Geomorphological Processes and the Development of the Lower Saint John River Human Landscape

GEOMORPHOLOGICAL PROCESSES AND THE DEVELOPMENT OF THE LOWER SAINT JOHN RIVER HUMAN LANDSCAPE

Pamela Jeanne Dickinson

Bachelor of Arts, University of New Brunswick, 1993 Master of Science, University of Maine, Orono, 2001

A Dissertation Submitted in Partial Fulfilment of the Requirements for the Degree of

Doctorate of Philosophy

in the Graduate Academic Unit of Geology

Supervisor(s): Dr. B.E. Broster, Department of Geology, Chair Dr. D.W. Black, Department of Anthropology

Examining Board: Dr. R. Miller, Department of Geology Dr. E.E. Hildebrand, Department of Civil Engineering Dr. P. Arpe, Department of Forestry

External Examiner: Dr. T.J. Bell, Department of Geography, Memorial University

This dissertation is accepted by the Dean of Graduate Studies

THE UNIVERSITY OF NEW BRUNSWICK

June 2008

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1+1 Canada ABSTRACT

The nature of human interaction with the landscape, both past and future, is an essential question for both geology and archaeology. Landscape elements are controlled in large part by long-term temporal processes and are recorded in the thick sedimentary deposits found within the lower Saint John River valley, New Brunswick.

A 67 m continuous core was recovered through drilling at Grand Lake Meadows, located at the junction of Grand Lake and the Saint John River, approximately 55 km south of Fredericton, New Brunswick. Sediment samples were collected from the core to identify stages of development of the marsh land area and surrounding environs since deglaciation. Analytical tests include particle size analysis and atterberg limit determination, loss-on-ignition, x-ray diffraction, and ion chromatography. Organic samples were also collected for radiocarbon dating, which allowed for the development of chronological control of changes in both the environmental and archaeological record.

The Grand Lake Meadows is interpreted as having evolved through four phases of development. Phase one starts with deglaciation and continues to ~11,500 BP.

Deglaciation began into a marine environment, which was undergoing desalinization due to pulses of fresh water from melting ice and retreating glaciers. Phase two began

-11,500 BP and continued until 8000 BP at which time there was major isostatic readjustment in the region. It was during phase two that the stratified Ancestral Grand

Lake was established. Phase three began ~8000 BP and continued until 3000 BP. Phase three represents an increased northern contribution of fresh water and the demise of

Ancestral Grand Lake. The lower Saint John River valley consisted of a fluvial dominated fresh water system, which likely initiated the down-cutting of the Reversing

n Falls gorge at the coast. During phase four, -3000 BP to present, marine water breached the Reversing Falls allowing saline water to penetrate into the lower Saint John River valley. This breaching at the falls led to the development of the modern river valley and

Grand Lake Meadows. This landscape reconstruction, which documented change in the sediment system, landscape morphology, depositional histories and chronology, examines possible linkages between geological events and human activity within the

Grand Lake Meadows system.

m ACKNOWLEDGEMENTS

I am extremely thankful for the assistance and patience of my supervisors,

Dr. Bruce Broster (Department of Geology UNB) and Dr. David Black (Department of

Anthropology UNB). I am indebted to both for sharing their interdisciplinary perspective on research and their encouraging words. Many thanks also to Dr. Ron Pickerill

(Department of Geology UNB), Dr. Randy Miller (New Brunswick Museum), Dr. Eldo

Hildebrand (Department of Civil Engineering UNB), Dr. Paul Arpe (Department of

Forestry UNB), and Dr. Trevor Bell (Department of Geography Memorial University of

Newfoundland).

There are many additional individuals who have in one way or another contributed to the present research. I would like to thank the faculty and staff in the

Department of Geology for their assistance and support during the preparation of my dissertation. I would also like to especially thank Dr. Suporn Boonsue, Dr. Tom Al and

Dr. Cliff Shaw. I would also like to thank my friends and fellow graduate students for their insights, wide ranging expertise and encouragement.

The present dissertation could not have been completed without the financial support provided by the Environmental Trust Fund, New Brunswick Geologic Survey,

Grand Lake Meadows Trust Fund, New Brunswick Museum and the Geological Society of America.

IV TABLE OF CONTENTS

Abstract ii Acknowledgements iv Table of Contents.... v List of Tables vii List of Figures viii List of Plates , xi

CHAPTER 1 INTRODUCTION 1 1.1 Objectives and Scope 4 1.2 Site Location 7 1.3 The Modern Environment 9 1.3.1 Overview of Late Quaternary Landform Development 15 1.3.2 Climate of the Lower Saint John River Valley 18 1.4 Bedrock Geology 23 1.5 Glacial History of the Lower Saint John River Valley 24 1.6 Physiography 37 1.6.1 Grand Lake Meadows 38 1.6.2 Major Geomorphological Events 40 1.6.2.1 Formation of a Glacial Lake 41 1.6.2.2 Formation of an Estuary 42 1.7 Previous Core Analysis in the Fredericton Area 43

CHAPTER 2 ARCHAEOLOGY OF THE LOWER SAINT JOHN RIVER VALLEY. 45 2.1 Culture History , 46 2.1.1 Palaeoindian Period (prior to 9000 BP) 46 2.1.2 Archaic Period (9000 to 2800 BP) 48 2.1.3 Maritime Woodland Period (2800 to 500 BP) 51 2.2 Archaeology of the Grand Lake Meadows 52 2.3 Spoken History of the Lower Saint John River Valley 53

CHAPTER 3 INVESTIGATION METHODS 56 3.1 Drilling and Coring 56 3.2 Laboratory Analysis - Procedures 67 3.2.1 Accelerator Mass Spectrometry Radiocarbon Dating 70 3.2.2 Laminae 72 3.2.3 Particle Size Analysis (Hydrometer) 73 3.2.4 Atterberg Limit Determination 74 3.2.5 X-Ray Diffraction Method 75 3.2.6 Ion Chromatography 76 3.2.7 Loss-on-Ignition 77 3.2.8 Natural Moisture Content 79 3.3 Results of Laboratory Analysis 80 3.3.1 Accelerator Mass Spectrometry Radiocarbon Dates 80 3.3.2 Laminae 81

v 3.3.3 Particle Size Analysis (Hydrometer) 84 3.3.4 Atterberg Limit Determination 86 3.3.5 X-Ray Diffraction 86 3.3.6 Ion Chromatography 92 3.3.7 Loss-on-Ignition 92 3.3.8 Natural Moisture Content 97 3.4 Interpretation of Laboratory Analysis 97 3.4.1 Accelerator Mass Spectrometry Radiocarbon Dates 99 3.4.2 Laminae 101 3.4.3 Particle Size Analysis (Hydrometer) 103 3.4.4 Atterberg Limit Determination 103 3.4.5 X-Ray Diffraction Method 104 3.4.6 Ion Chromatography 107 3.4.7 Loss-on-Ignition 116 3.5 Statistical Analysis... 124 3.5.1 Spearman Rank Correlation 125 3.5.2 Agglomerative Hierarchical Clustering 130 3.5.3 Discriminant Analysis 132

CHAPTER 4 RESULTS 138 4.1 Facies Model of Deposition 138 4.2 Stratigraphic Units 144

CHAPTER 5 DISCUSSION 148 5.1 Glacial History 149 5.2 Climate Determined from LOI Analysis 152 5.3 Prehistory and Human Habitation 153

CHAPTER 6 CONCLUSIONS 157 6.1 Post Glacial Geological Interpretations of the Grand Lake Meadows Region.. 157 6.2 Implications of the Geological Interpretations for Archaeological Research.... 168 6.3 Sea-level Rise 172

References 175

Appendix I: Grand Lake Meadows (GLM-01) Core Log Appendix II: Particle Size Analysis (Hydrometer Results) Appendix III: Atterberg Limit Results Appendix IV: X-Ray Diffraction Results Appendix V: Loss-on-Ignition Results Appendix VI: Ion Chromatography Results Appendix VII: Accelerator Mass Spectrometry Radiocarbon Dates

Curriculum Vitae

VI LIST OF TABLES

Table

2.1 Precontact archaeological sites identified within the Grand Lake Meadows 53

3.1 Details of AMS radiocarbon-dated samples from the GLM-01 core 81

3.2 Dissolved solids-salinity relationships 108

3.3 The 11 main salt ions of seawater 108

3.4 Chloride concentration (mg/L) from locations along the lower Saint John

River 114

3.5 Samples extracted from the GLM-01 core for coal identification 120

3.6 Correlation between LOI and sand, silt, clay and percent silt plus clay 128

3.7 Correlation between chloride and clay, and chloride and silt 128

3.8 Correlation was noted between bromide and clay, and bromide and silt.... 128 3.9 Classes and object number produced on the dendrogram from the clustering analysis 130 4.1 Stratigraphy and interpreted stratigraphy produced from the GLM-01 core 144

Vll LIST OF FIGURES

Figure

1.1 Location of study area 3

1.2 Delineation of the Grand lake Meadows area with drilling location marked 8

1.3 Physiographic regions of New Brunswick 10

1.4 Area where surficial geological research has been completed 17

1.5 Maine, USA, Quaternary relative sea-level data 28 1.6 Landsat satellite image highlighting the incursion of early marine water into central New Brunswick at 80 m, with delta elevations labeled 32

1.7 Three-dimensional 80 m marine inundation into central New Brunswick 33

1.8 New Horton and Bocabec Lake, New Brunswick 36

3.1 Arial photograph with drilling location marked 58

3.2 Stratigraphic model across the two major rivers within the Grand Lake Meadows; Saint John River to the west of the drill location and the Jemseg River to the east 62

3.3 Summary of results of laboratory testing with dots depicting laminae normalized per 610 mm compared with depth 83

3.4 Summary of results of hydrometer tests depicting the percent each of sand, silt and clay with depth 85

3.5 Summary of results of laboratory testing depicting variation of liquid limit, plastic limit and natural water content with depth 87

3.6 Summary of results X-ray diffraction testing depicting variation in mineralogy with depth 88

3.7 Summary of results depicting vivianite location with depth 91

3.8 Summary of results of the ion chromatography tests depicting the chloride content (mg/L) with depth 93

3.9 Summary of results of the ion chromatography tests depicting the bromide content (mg/L) with depth 94 3.10 Summary of results of the ion chromatography tests depicting the chloride and bromide ratio with depth 95

3.11 Summary of results of the loss-on ignition tests depicting the amount of organic material with depth 96

3.12 Summary of results of the natural moisture tests with depth 98

3.13 Summary of results of each of the measured dates (including the confidence interval to 1 standard deviation) with depth 100

3.14 Location map where chloride concentrations for precipitation data has been tabulated for twelve stations throughout New Brunswick by the New Brunswick Department of Environment 113

3.15 Location map depicting area in New Brunswick underlain by coal in the bedrock 118

3.16 Summary of results depicting no significant difference in the temperature at which the coal from Salmon Harbour and Fire Road Mine ignited 121

3.17 Summary of results depicting that the coal from Salmon Harbour and Fire Road Mine were both completely burned off after ~1.5 hours at 500°C 123

3.18 Connected scatter plot of LOI 126

3.19 Connected scatter plot of chloride/bromide ratio 127

3.20 Dendrogram with eight variables (depth, gravel, sand, silt, clay, LOI, chloride and Bromide) 131

3.21 Five distinct facies identified within the core 133

3.22 Discriminant analysis with two quantitative observations relating to soil depositional environment (chloride and bromide) and depth, as plotted against five qualitative systems (floodplain, fluvial, lake, marine and deglacial till) 134

3.23 Discriminant analysis with three quantitative observations relating to hydrology and depositional environments (gravel, sand and percent silt plus clay) and depth, as plotted against five qualitative systems (floodplain, fluvial, lake, marine and deglacial till) 136

3.24 Discriminant analysis with four quantitative observations (depth, percent silt plus clay, LOI and chloride/bromide ratio), as plotted against five qualitative systems (floodplain, fluvial, lake, marine and deglacial till) 137

IX 4.1 Facies model of deposition depicting the stratigraphy and interpreted stratigraphy for the GLM-01 core 139

4.2 Summary of results of laboratory testing of core, a) stratigraphy, b) AMS dates, c) chloride/bromide ration, d) loss-on ignition and e) grain size 141

6.1 Archaeological cultural history in the context of the stages of deposition within the Grand Lake Meadows with the radiocarbon dates 169

x LIST OF PLATES

Plate 3.1 Drill at core location within the Grand Lake Meadows 60

3.2 Lantech Drilling Services Inc. track mounted hollow stem auger drill at

drilling location 64

3.3 Split spoon with an inside diameter of 35 mm and length of 600 mm 65

3.4 Shelby tubes with an inside diameter of 73 mm and length of 600-750 mm 66

3.5 Core extracted into split PVC pipe 68

3.6 Core lengths split down the central axis using a guitar string 69

3.7 Laminations on wet sediment in the GLM-01 core 82

3.8 Photograph of the mineral vivianite at 19 m depth below surface 89

3.9 Photograph of the mineral vivianite found in association with organics at

40 power, 2.5 m depth below surface 90

3.10 An example of a fluid structure found throughout the core 102

3.11 Coal was confirmed using the Scanning Electron Microscope in one sample from a depth of 7.8 m dbs 119

XI CHAPTER 1

INTRODUCTION

Geological investigations provide the key to interpreting the sediment record and recognizing landscape change within a region. This information provides a means for reconstructing ancient landscapes and palaeoclimatic regimes, necessary to interpret precontact human subsistence activities, migration routes, settlement location, and local and regional land use patterns, as well as an understanding of site formation, preservation and erosion. Geological processes shape, and potentially bias, our interpretation of the archaeological record. An understanding of the postglacial geological and environmental development of an area is vital to reconstructing the timing and spatial distributions of archaeological remains and past human activities.

Estuaries, such as that found in the lower Saint John River valley, preserve a deep

Holocene sediment sequence. Additionally, they offer opportunities for the preservation of organic remains, which allows for the development of a chronological sequence for the region. Estuaries are subject to a combination of riverine, coastal and terrestrial environmental factors. At any given location the relative influence of each will vary through time, creating a highly dynamic geoarchaeological context, which is distinctive from non-estuarine environments.

Environmental change is an especially important characteristic within an estuarine environment, often occurring on a multiplicity of time-scales, from the astronomically predictable tidal cycles, springtime cycles, equinoxial cycles to longer-term astronomically related cycles. Additionally, there is also the influence of longer-term

1 climatic and sea-level changes, as well as sudden events arising from storm surges and floods that, if critical thresholds are crossed, may trigger longer-term changes. Estuaries that contain evidence of clearly defined environmental changes, which can be precisely dated, hold the contexts in which to investigate the relationship between environmental and landscape change, and to determine how that may have impacted human population in the region.

Concern for the increased frequency of extreme climate events is highly relevant to contemporary society. Reconstructing the past frequency of extreme events (i.e. droughts and extreme warm periods) enables modern society to anticipate and plan for future climate change. Modern instrumental records of climate span only the last two centuries; therefore, palaeoenvironmental methods are required to assess baseline conditions within terrestrial and aquatic ecosystems, and are used to evaluate past climate and environmental changes. Sediment can be used to infer regional climatology and ecology because it can accumulate in an ordered manner, deposit rapidly, and contain physical, chemical, and biological information about past environmental conditions.

When deep sediment sequences are dated reliably using radiocarbon and/or other methods, the timing of past environmental changes can be estimated. The study presented here consisted of the extraction and analysis of a sediment core record from the

Grand Lake Meadows region (Figure 1.1), within the lower Saint John River valley, southcentral New Brunswick.

2 Vi £ <& Prince Edward Island U.S.A. New Brunswick # lFredericton * Study areaT

Saint John

Nova Scotia %

Figure 1.1: Location of study area.

3 1.1 Objectives and Scope

This project is centered around prehistoric landscape and landscape change with a focus on human and natural interactions from a geological perspective. More specifically the research focused on reconstructing the geomorphic character of the Grand Lake

Meadows and its setting, the lower Saint John River valley, and how this environment may have affected past human occupations within the region. Analytical methods follow from geoarchaeological research and the types of fundamental information that geoarchaeology can provide to advance regional landscape interpretation.

Sediment cores hold information that allows for an understanding of the composition and alteration of landforms, as well as the processes that may have shaped and changed them. There are a number of natural influences that can cause a landscape to change, such as climate, relief and drainage system changes. During the early

Holocene the lower Saint John River valley was particularly influenced by events associated with glacial, periglacial and interglacial environments. In this region there have been fluctuations in temperature throughout the Holocene, which would have led to climatic, soil and vegetation changes (Mott et al. 1986; Levesque et al. 1993a, 1993b;

Mayle et al. 1993a; Levesque et al. 1994). This study involves the analysis of a sediment core extracted from the Grand Lake Meadows, lower Saint John River valley. The study builds on reconstructed climatic models (Levesque et al. 1993b; Mayle and Cwynar

1995a), as well as interpretations of the late glacial history of the region (Seaman 2006) by recognizing and deciphering geologic events that impacted landform formation and change.

4 Control for this study was based on continuously drilling and sampling the thick glacigenic sequence found within the Grand Lake Meadows. The drilling location was chosen based on previous core logs obtained from the Province of New Brunswick's

Department of Transportation (DOT), which crossed the lower Saint John River at the

Grand Lake Meadows and the Jemseg River at Jemseg. The lithology, physical properties and organic content of the sediment from the core were analyzed in order to understand more about the depositional mechanisms and environments of these units, particularly the glacial marine and glacial lacustrine environments. Accelerator mass spectrometer (AMS) radiocarbon dates were obtained from organic material, which allowed for chronological control of the upper half of the core. Based on the interpreted environments of deposition, coupled with chronological control, a depositional history has been constructed. Insights into the timing, extent and formation of an inland sea, glacial lake, floodplain, and an estuary are postulated.

A detailed geomorphological study of the lower Saint John River watershed is needed to delineate the palaeoenvironmental controls on Wisconsinan deglaciation and

Holocene human occupation of the region. The traditional approach to palaeoenvironmental research in the Maritime Provinces has been macro environmental, consisting of broad temporal and spatial vegetation histories based primarily on pollen analysis (Mott 1975; Mott et al. 1986; Cwynar et al. 1994) and the impact of the Younger

Dryas climatic event (Levesque et al. 1993a, 1993b; Mayle et al. 1993a). This research is commonly supplemented by investigations of regional geomorphological trends. Such investigations typically include crustal downwarping and isostatic rebound causing changes in sea-level (Stea et al. 1994, 1998), as well as the formation of glacial features

5 such as delta systems, glacial striae and till dispersal trends (Pronk and Seaman 2001;

Seaman 2006). However, palaeo-macroenvironmental research frameworks may be difficult to apply or problematic at finer temporal and spatial scales.

This project allowed for the development of a comprehensive landscape reconstruction for the Grand Lake Meadows region, and addresses how particular geological/environmental events may have impacted archaeological situations, which may have facilitated or inhibited early human occupation in the region. The timing of postglacial, early human occupation and habitation for most of New Brunswick is as yet unknown. However, much research has been completed regarding the earliest culture period, the Palaeoindian culture period (~11,000 - 9000 BP), in adjacent Canadian provinces and American states (MacDonald 1968; Granily 1982; Keenlyside 1985; Spiess and Wilson 1987; Davis 1991; MacCarthy 2003).

The primary focus of this project was to understand the nature and development of the lower Saint John River valley post-glaciation to present day. From this it is possible to gain an understanding of how human occupation and mobility may have been influenced by physical changes within the valley. Specific objectives of the research included:

1. to analyse the causes and events leading to deposition and accumulation of the

sedimentary units and development of a facies model of deposition;

2. to establish a dating framework for the Grand Lake Meadows, found within the

lower Saint John River valley; and

3. delineate the relationship between palaeo-landscapes and occupation by pre-

contact peoples.

6 Analytical data were collected that could be used to place 'traditional' archaeological research into a wider context, as well as answer some of the geological questions relating to the lower Saint John River valley throughout the Holocene.

Following the fieldwork, some selection was required in terms of the range of analytical techniques used. Analysis was constrained to conventional lithological techniques of particle size analysis, atterberg limit determination and moisture content, ion chromatography, loss-on-ignition, X-ray diffraction, and independent chronologies were established through AMS radiocarbon dating.

1.2 Site Location

The Grand Lake Meadows is located in southcentral New Brunswick in the lower

Saint John River valley at the confluence of Grand Lake and the Saint John River. The

Grand Lake Meadows is defined for the purposes of this study in a similar manner as proposed by Washburn and Gillis Associates Ltd. (1996, pp. 2-3) in their preliminary environmental impact assessment on the then-proposed, new Trans-Canada Highway.

Washburn and Gillis (1996) defined the area as being bounded on the east by the Jemseg

River and on the north by various bodies of water including Grand Lake, Back Lake,

Maquapit Lake, French Lake and two extensive thoroughfares, the Blind Thoroughfare and the Lower Thoroughfare (Figure 1.2). The Saint John River represents the southern and western extent of the Grand Lake Meadows region, with the northwestern limit defined by a road that connects McGowans Corner to Lakeville Corner. The total region encompasses approximately 500 hectares (Choate 1973), consisting primarily of a broad flat floodplain and wetland meadow, with elevations ranging from just above sea-level to

7 • ^renchvy^JTsr^&i- Blind Thoroughfare ^ \- Maquapit-^^'^., :;^ake {jTl^g """ , JV " * ' • Lower Thorouehfare

Figure 1.2: Delineation of the Grand lake Meadows area with drilling location marked (base map Grand Lake 21 G/16, Edition 6, Survey and Mapping Branch, Department of Energy, Mines and Resources, 1980).

8 a height of 160 metres in the upland areas. The Grand Lake Meadows is divided by

Queens and Sunbury counties.

1.3 The Modern Environment

The Saint John River as a whole, rises on the border of the Province of Quebec and State of Maine at an elevation of 480 m asl and flows south for 730 km to the Bay of

Fundy (Thibault et al. 1985). The river drains approximately 55,000 km2 (Hustins 1974;

Thibault et al. 1985), with over 90% of the lakes (greater than 20 ha in extent) occurring in the lower Saint John River valley (Hustins 1974). Approximately one-third of the province is occupied by the New Brunswick lowlands (Figure 1.3), forming the eastern and central portions of the province. The Saint John River flows through this low-lying basin for more than 100 km, with the portion of the river lying in the central lowland being subject to extensive spring floods.

Grand Lake is located on the northeast side of the Saint John River, approximately 40 km south of Fredericton. At 16,500 hectares, Grand Lake is New

Brunswick's largest inland body of water. The lake drains through the Jemseg River and the Grand Lake Meadows into the Saint John River. This region hosts rich, temperate, abundant, deciduous forest locations, freshwater marshes, freshwater streams and salt and brackish marshes. The significance of the Meadows in the lower Saint John ecosystem has been recognized by three official designations:

• Grand Lake Meadows Protected Area, a 11,617 hectare site within the

Meadows, officially established by the New Brunswick Ministry of

Natural Resources and Energy in May, 2000;

9 Nova Scotia

Figure 1.3: Physiographic regions of New Brunswick (after Bostock 1970).

10 • Portobello Creek National Wildlife Area, a 1970 hectare reserve near the

Saint John River at Oromocto, just south of Fredericton; and the

• Lower Saint John River (Sheffield/Jemseg) Important Bird Area; Bird

Studies Canada with Bird Life International and the Canadian Nature

Federation identify the Oromocto section of the Saint John River as an

Important Bird Area of Canada

(www.gnb.ca/0078/publications/OurHeritage-e.pdf).

The Grand Lake Meadows is unique as it provides a complex setting for migrating waterfowl, aquatic and terrestrial plants and animals, and unique associations of hardwood swamp vegetation with southerly affinities (Choate 1973). Today the region has the wannest climate in New Brunswick (Dzikowski et al. 1984; NBDNRE 1998, p. 12). Due to the number of large water bodies the region acts as a heat sink producing the highest average temperatures and longest growing season in the province (NBDNRE

1993). During the warm summer months the large water bodies store heat and then release it in the fall, also extending the frost-free season for the region

(http:www.gnb.ca/0078/publications/OurHeritage-e.pdf). Therefore, some of the vegetation species found in the province are almost exclusive to this region, in particular ironwood, basswood, butternut, white ash, green ash, and silver maple (NBDNRE 1993).

The study area is also composed of additional environmental features that influence growth and development of tree species. Coarse, alluvial deposits consisting mainly of riverbank sediments support trees such as white pine, bur oak, green ash, butternut and silver maple; however, in areas that are flooded less frequently, sugar maple, red maple, basswood, ironwood, white ash and red oak stands are found

11 (NBDNRE 1993). Finally, on the well-drained upland soils mixed wood stands of red spruce, hemlock, red maple, white birch and trembling aspen are common (NBDNRE

1993). Anthropogenic disturbance, particularly agriculture and forestry, has altered the original forest considerably (NBDNRE 1993).

From a review of available maps obtained for the area, it appears that the primary historical land transportation routes have always been situated along the well-drained levee to the south of the Grand Lake Meadows (DND 1938; ASE 1957/58a, 1957/58b;

NBDEMR 1980; GSC 1880, 1884). The earliest maps available, produced by the

Geological Survey of Canada in 1880 and 1884, indicate that a portion of what is now the

Trans-Canada Highway Route 2 through the meadows was then used as a road. This road extended to approximately the area currently known as The Intervale on the southwest portion of the Grand Lake Meadows (Figure 1.2). At this time Highway 690, from

McGowans Corner to Lakeville Corner, was also shown to have been in existence, crossing at Fulton Island as it does today. At low water, the remains of bridge pilings are still visible at the western tip of the island, immediately east of the'current bridge.

By 1958, the main road through the Grand Lake Meadows had become part of the

Trans-Canada Highway. In addition, a ferry connection was added linking The Intervale to Upper Gagetown, on the southern shore of the Saint John River. This ferry connection remained in service until the end of the 20th Century, when a bridge was constructed across the Saint John River approximately 3 km downstream from the ferry crossing.

Throughout the 20l Century, the primary land transportation routes remained unchanged; however, at the end of the 20th Century, a new route was proposed through the Grand Lake Meadows with the construction of a new Trans-Canada Highway, known

12 as the #2 Highway. In addition to the previously mentioned bridge built across the Saint

John River, a new bridge was built at Jemseg, just downstream from the existing crossing. An elevated four-lane highway was also constructed to the north of the existing

Trans-Canada Highway and joined with the existing highway at the new bridge crossing to the east of The Intervale.

The landscape of the Grand Lake Meadows has been impacted anthropogenically throughout the historic period. Such impacts have affected cultural resources located within the region. A number of recent archaeological mitigative excavations have been completed to allow for the construction of the new #2 Highway through the Meadows region, for example the Jemseg Crossing, Grand Lake Meadows and Swan Creek Lake

East archaeological projects (Blair 1997; JWEL 2003, 2004). To understand the impact of changing land-use patterns throughout the Holocene better models of estuarine sedimentary deposits and evolution are needed.

The Saint John River flows into the Bay of Fundy, an arm of the Gulf of Maine system, which, in modern times, has some of the highest tidal amplitudes in the world, reaching 16 m at the head of the bay. At high tide, the force of the ocean overwhelms the flow of the river. In modern times, the lower reaches of the river have stratified layers of fresh and salt water. The upper two-thirds of the Saint John River estuary, including

Grand Lake, is entirely freshwater, while the lower one-third of the estuary is increasingly saline downstream as a result of incoming tides (Messieh 1977). During the

Holocene, when sea-level was at its lowest, the Saint John River above the Reversing

Falls contained exclusively freshwater, which flowed over a significant waterfall into the

Bay of Fundy (Flaherty 1989). The breaching of the sill at the mouth of the Saint John

13 River, accompanied by a rising tidal sea, was a threshold event that allowed for the development of anadromous fish runs into the river.

Anadromous fish would have impacted early food resources that were found in the lower river valley and could have included the addition of striped bass, freshwater eel, white perch, Atlantic tomcod, Atlantic salmon, sturgeons, gaspereaux, and shad.

Additionally, a number of marine fish may also have been found such as spiny dogfish,

Atlantic menhaden, and red hake (Meth 1971). Such fish were historically, and still are today, used by people who inhabit or visit the lower Saint John River valley, and have supported fisheries to modern times. Squires (1972, pp. 73-74) suggests that almost all of the freshwater and anadromous/catadromous fish that occur within the lower Saint John

River can be caught in the Grand Lake region.

The formation of the floodplain is a salient feature of the modern lower Saint John

River valley. When large amounts of water are released into the river, such as during the spring melt of snow, discharge into the Bay of Fundy is restricted by a narrow gorge at the mouth causing the river to back up and flood. This annual spring flooding has led to the development of a broad, flat floodplain that has enhanced agricultural potential for the region.

The ecological productivity of the lower Saint John River valley is significantly different from the upper and middle reaches of the river due to the influx of marine waters, the constriction of the river at its mouth, and the distribution of water resources that affect local climate. The region contains more than 165 plants with food potential,

37 plants with known medicinal uses and 28 plants that can be used for making tools

14 (Blair 2004, p. 138); therefore, the environmental productivity of the lower Saint John

River valley would have been very attractive to early people in the region.

The responses of river sediment systems to changes in land-use are conditioned by a complex interaction of factors, such as climate, drainage area, relief, type of sediment, as well as the vegetation and cultural histories of individual catchments. It is often important to discriminate between the effects of human activity, climate and other natural factors, and as such, a need for greater chronological precision is required. In order to be able to describe changes in any environment, dating is essential to determine rates of change as well as to place events in a geological or archaeological context.

Research that emphasizes the role of anthropogenic factors, especially since the advent of

European agriculture, focuses on the effect of people in clearing woodland and creating agricultural landscapes, which modern analogues show can have dramatic hydrological effects often leading to substantially increased soil erosion and thus sediment supply within the water systems (Waters 1995; Baron et al. 2002; Allan 2004). However, climatic parameters such as increase in temperature, changes in frequency and intensity of storms, variation in sea-level and precipitation also affect river regimes (Hare et al.

1997; Westmacott and Burn 1997). Finally, major hydrological events such as the change from a freshwater to an estuarine environment would greatly impact the lower

Saint John River ecosystem.

1.3.1 Overview of Late Quaternary Landform Development

The surficial geology of the lower Saint John River valley is located within the

New Brunswick Lowlands, a portion of the Maritime Plain that stretches around the coast

15 of New Brunswick (Bostock 1970). This region is a large, flat to gently undulating, low elevational (185 m asl) plain. Several events made their marks on the landscape, with the region having been sculpted by glaciation, marine and lacustrine submergence, isostatic rebound, alluviation, stream and river erosion and weathering (Rampton and Paradis

1981a, 1981b).

As the glacial ice from the Wisconsinan glaciation moved across New Brunswick it modified valleys such as the Saint John River valley, eroding rock and carrying its debris within the ice for kilometres (Seaman 2006). All the unconsolidated sediments that cover most of New Brunswick today are primarily products of this last glaciation.

Some of these sediments were deposited directly from the glacial ice as a cover of till, while other finer sediment washed into the sea or accumulated in meltwater streams and glacial lakes.

A considerable amount of surficial geological mapping has been expended on the southeastern and southwestern portions of New Brunswick (Lee 1957; Gadd 1968;

Brinsmead 1974a, 1974b; Lohse 1974a, 1974b; Brinsmead and Finamore 1977; Belanger

1978; Seaman 1982; Thibault 1983; Chiswell and Long 1989; Foisy and Seaman 1989;

Foisy and Prichonnet 1991; Balzer 1992; Stumpf and Seaman 1997; Pronk 1998; Allaby et al. 1999) (Figure 1.4). However, little research has focused on southcentral New

Brunswick or the lower Saint John River valley (Lee 1957; Belanger 1978).

Additionally, much of the glacial/deglacial research has focused on areas outside the

Saint John River valley (Gadd 1973; Gauthier 1979, 1980; Rampton and Paradis 1981a,

1981b; Seaman 1985, 1990, 2000; Thibault et al. 1985; Broster and Seaman 1991;

Seaman et al. 1993; Stumpf 1995), with little research directed within the lower portion

16 Figure 1.4: Area where surficial geological research has been completed is indicated by shading.

17 of the valley itself (Seaman 1982, 1988b, 1989a, 1989b, 1991; Rampton et al. 1984;

Nicks 1988; Foisy and Seaman 1989).

Sediment storage and entrainment along the lower Saint John River valley varies in response to valley geometry, available sediments, and topographic controls. The valley is broad and flat in the Grand Lake Meadows region. Significant input is available from the seven large tributary watersheds (Blair 2004, p. 136), resulting in periodic increased discharge and high sediment delivery rates to this area. The sedimentary history of the Grand Lake Meadows area is one of long-term aggradation.

Alluvial stratigraphy can be shaped by a wide variety of processes, including lateral stream migration, avulsion, in-channel deposition, levee growth, splay and overbank deposition, and other factors. In addition, the surficial geomorphic evolution of the valley system is shaped by both external and internal controlling factors, including sediment characteristics, vegetation, and changes in catchment hydrology and sediment yield through time. The present study concentrates on recognizing the large scale, fundamental behaviours relating to the key surficial processes in a framework that explains the fundamental nature of the lower Saint John River valley.

1.3.2 Climate of the Lower Saint John River Valley

The current climate in New Brunswick is characterized by peak rainfall between

May and August with average total annual accumulations of 844 mm. Of this, snowfall totals an average of 295 cm annually with peak amounts in January and February.

Temperatures vary considerably with the annual maximum mean temperature in August and the minimum in January. The average annual temperature is 11° C for the maximum

18 and -1 °C for the minimum (http://atlantic-webl.ns.ec.gc.ca); however, over the past

13,000 years the regional climate has fluctuated significantly. (Levesque et al. 1993b;

Mayle and Cwynar 1995a).

Late glacial climate reconstructions for New Brunswick, between 14,000 and

10,000 BP, describe a rapidly changing environment (Mott 1975; Mott et al. 1986;

Leveque et al. 1993a, 1993b, 1994, 1997; Mayle et al. 1993a; Cwynar et al. 1994; Mayle and Cwynar 1995a). A unique feature of the climate in New Brunswick at this time is the exceptionally steep north to south temperature gradient (Levesque et al. 1997); as a result, a higher degree of richness and diversity of flora occurs around the more southerly lakes, such as Grand Lake. It has been suggested that the strong north to south temperature gradient was related to the proximity of the melting Laurentide ice sheet

(Levesque et al. 1997), which may have had an effect on the environment of New

Brunswick as late as 8000 BP (Knox 1983).

In New Brunswick at present, a mean average summer surface water temperature difference of less than 2° C occurs in lakes over a distance of 250 km; however, during the post-glacial warm periods the difference was often as high as 10° C (Levesque et al.

1996). These differences in temperature were likely responsible for the development of plant and animal species boundaries affecting early human habitation location. This north to south temperature gradient also affects the total growing degree-days. Colpitts et al. (1995) have divided the province into four climatic regions based on the growing degree-days, which are characterized by the length and warmth of the growing season, and the amount of local precipitation. These regions include:

19 1. the Grand Lake basin of the New Brunswick Lowlands, which has >1800

annual growing degree days;

2. the southern part of the province including the central and southern New

Brunswick Lowlands and parts of the St. Croix Highlands, which has 1600 to

1800 annual growing degree days;

3. the northern half of the province and along the coast of the Bay of Fundy,

which have 1400 to 1600 annual growing degree days; and

4. the Kedgwick and northern Miramichi Highland regions, which have 1200 to

1400 annual growing degree-days.

The vegetation of New Brunswick is part of the Southern Mixed Forest Region that encompasses central and eastern Canada (Ontario-Manitoba border on the west with the Maritimes and Atlantic coast on the east). In particular, the province is part of the sub-class called the Acadian Forest Region, which is associated with deciduous and boreal forests (Clayden 1999).

Throughout the Acadian Forest Region, early historic agricultural settlement, which includes large-scale lumbering and swidden agriculture, has largely altered the pre-

European composition of the forests. Due to poor soil conditions and uneven topography, many of these early agricultural fields have now been abandoned and forest re-growth is underway (Clayton et al. 1977). The soils of this region are classified by

Clayton et al. (1977, p. 120) as podzolic, which refers to the "well to imperfectly drained mineral soils with characteristics and features that developed under the influence of forest and heath vegetation". More specifically, the soils of the Grand Lake Meadows area are

20 known as "interval" soils, ranging in drainage from very poor and poor to well

(http://res.agr.ca/cansis/).

Palaeoenvironmental reconstructions for the Maritime Provinces and eastern

United States are mainly based on palynological studies (Davis 1969; Mott 1975, Davis and Jacobson 1985; Mott et al. 1986; Levesque et al. 1993a, 1993b, 1994, 1997; Mayle et al. 1993a; Cwynar et al. 1994; Mayle and Cwynar 1995a, 1995b). Fossil pollen grains suggest that the Laurentide glacier began to retreat by approximately 13,000 BP, accompanying a climatic warming. This warming trend continued until just prior to

11,000 BP when another cold event occurred, named the Killarney Oscillation (Levesque et al. 1993b). This cold period, represented by a cooling of approximately 8° to 12° C

(Levesque et al. 1994), lasted for approximately 300 years. The subsequent warming period, the Allerod period, was of short duration, followed by the more severe Younger

Dryas cooling event that began shortly after 11,000 BP and returned the New Brunswick climate to near glacial conditions. The Younger Dryas remained until approximately

9500 BP, its end marking the beginning of the Holocene and a subsequent rapid climatic warming (Cwynar et al. 1994).

The shift in climatic trends and subsequent changes in pollen spectra are clearly demonstrated in regional pollen diagrams. Pollen diagrams developed by Davis (1969),

Mott (1975), Mott et al. (1986), Cwynar et al. (1994), and Levesque et al. (1994) indicate:

• by 13,000 BP a tundra environment dominated the Maritime region and the

landscape became vegetated by grasses, shrubs and herbs;

• by 12,600 BP birch, poplar and willow became more abundant;

21 • by 12,000 BP the environment became open spruce Maritime Woodland with

shrub birch;

• from 11,000 to about 10,000 BP spruce started to decline as a cool-climate

tundra environment increased; and finally

• after 10,000 BP the climatic and vegetative conditions of today began to

develop across the province.

These climate changes would have had a strong effect on the alluvial chronologies of the Saint John River. The amount of channel and/or valley alluviation or erosion changes as climate conditions change. Commonly, alluviation increases after an environmental shift to drier or warmer conditions, whereas erosion or entrenchment may become more prominent after a shift to wetter or cooler conditions (Knox 1983;

Levesque et al. 1994). This relationship is likely related to a vegetation decrease, and therefore, higher sediment yields during dry environmental episodes such as the Younger

Dryas cooling event or the Killarney Oscillation (Levesque et al. 1994).

It is difficult to correlate palaeoecological work with perceived human land-use models. However, climatic changes associated with the Younger Dryas would have impacted human resource procurement strategies as the spruce populations in the

Maritimes shifted southward and the open tundra vegetation, including sedges, expanded

(Newby et al. 2005, pp. 145-147). From these palaeoecological models the movement of early hunter/gatherers/fishers is generally linked to changing environmental conditions that would have also effected the movement of caribou herds. Newby (2005, p. 151) suggests that the Younger Dryas vegetation patterns would have been suitable for long distance migrating caribou, which early people would have followed.

22 1.4 Bedrock Geology

The headwaters of the Saint John River, within New Brunswick, are located in the northwestern portion of the province in the Chaleur Uplands. This low, gently undulating land surface is largely underlain by Early Palaeozoic, marine clastic calcareous and argillaceous sedimentary rocks consisting of shale, sandstone and limestone. However, the bedrock geology of the region also includes small areas of gypsum and silicic to mafic volcanic flows, tuffs and intrusive rocks (Potter et al. 1979).

The Saint John River follows a course through the Miramichi Highlands, part of the New Brunswick Highlands, flowing from northwestern to southeastern New

Brunswick. This rugged region is underlain by complex geological formations comprised chiefly of Lower Palaeozoic metasedimentary and calcareous sedimentary bedrock

(Potter et al. 1979; NBDNRE 1998). Mafic and felsic igneous rocks have significantly intruded these geological formations, which creates an irregular topography.

Southeast of the Miramichi Highlands (Figure 1.3), the Saint John River enters the New Brunswick Lowland portion of the Gulf of St. Lawrence Plain. The river broadens throughout this region and is enclosed by extensive undulating floodplains.

Surface relief within the region is related to the underlying, eroded Carboniferous coal- bearing coarse-grained clastic sediments, consisting predominantly of sandstone and conglomerates (Clark 1962; Gadd 1973; Ferguson and Fyffe 1985) and calcareous and non-calcareous, sedimentary rocks of Upper Palaeozoic age (McLeod et al. 1974;

Colpitts et al. 1995). Incision by the river and its tributaries resulted in a local relief of up to 150 m (Rampton et al. 1984). The Saint John River valley portion of the lowlands,

23 consist primarily of siliciclastic sediments and formations of grey lithic and feldspathic sandstones (Colpitts et al. 1995).

Further southward, the Saint John River passes through the southern portion of the New Brunswick Caledonia Highlands, which has a relief of 50 to 100 m (Rampton et al. 1984). These highlands are underlain by intensely deformed Upper Precambrian sedimentary, volcanic and intrusive rocks and Cambrian marine sediments, which are in places overlain by Carboniferous sediments (Ferguson and Fyffe 1985). These geologically complex rocks create a rugged topography that includes interbedded felsic and mafic volcanic rock, areas of siliclastic sedimentary rocks composed of calcareous red mudstones, red sandstones and conglomerates, as well as granitic and slightly calcareous sedimentary rocks (Colpitts et al. 1995).

1.5 Glacial History of the Lower Saint John River Valley

Significant to the modern structure of the lower Saint John River is the late

Pleistocene/early Holocene geology of the region. Climate changes resulted in a cycle of cold and warm periods, causing the sea-level to rise and fall as large amounts of water were alternatively locked away in and released from large ice sheets. The only unglaciated portions of the Maritime Peninsula (the Maritime Provinces, Quebec and

Maine) were offshore islands and peninsulas that are now part of the continental shelf, which include the Georges Bank and Sable Island (Pielou 1991; Shaw et al. 2006). Land- based glacial ice incurred a rapid decrease in ice volume between 19,000 BP (Yokoyama et al. 2000) and 18,000 BP (Shaw et al. 2006). Ice retreat in the southwest was mainly by

24 calving along embayments where an early ice stream occupied the Bay of Fundy/Gulf of

Maine region (Shaw et al. 2006).

Just prior to this time sea-level was significantly lower, as much of the world's freshwater was locked up in glacial ice, resulting in a low eustatic sea-level. At this time sea-level in the Bay of Fundy was up to 60 m lower and consisted of a broad open plain.

A land bridge connected Prince Edward Island with the mainland (Scott et al. 1987), and was referred to by Keenlyside (1983, 1991) as "Northumbria". The Fundian Moraine, mapped by Drapeau and King (1972) and Fader et al. (1977) would have become a linear positive feature indicating the location of ice termination. The Fundian Moraine crosses the Scotian Shelf, extending from the northern Georges basin in the Gulf of Maine, east to Roseway Basin. Todd et al. (1999) suggest that this glacial feature was completely transgressed during the late Wisconsinan-Holocene rise in sea-level, existing as an island on Browns Bank during the final stages of this marine transgression.

During the Late Wisconsinan New Brunswick was glaciated by southerly, to southeasterly, flowing glaciers (Lee 1957; Gadd 1973; Thibault 1981; Rampton et al.

1984; Seaman 1989a, 2004, 2006; Seaman et al. 1993). However, shortly after

14,000 BP (Borns 1963) the thickness of the ice started to decrease by means of regional ice stagnation and down-wasting (Seaman 1982, 2004). Finite dates for deglacial and post-glacial organic material found in New Brunswick have been tabulated by Rampton et al. (1984), and indicate that deglaciation of New Brunswick occurred between 14,500 and 10,000 BP. Organics overlying marine sediments have been dated from near Saint

John and indicate an active glacial ice margin terminating about 13,400 BP (Gadd 1973;

Rampton et al. 1984; Nicks 1988), establishing the time of glacial retreat of ice from the

25 Saint John area. Retreat of the ice front was time-transgressive in a southeast to northwest direction (Seaman 2004, 2006). Ice retreat led to the deposition of till, ice- contact deposits and glaciofluvial deposits (Gadd 1973; Seaman 2006).

Deglaciation and marine submergence were contemporaneous events (Lougee

1953; Bloom 1963; Borns 1963; Borns and Hagar 1965; Schnitker 1974; Stuiver and

Borns 1975; Seaman 1982). Bones and shells found along the coast of New Brunswick indicate marine sediments dating between 13,400 and 12,000 BP (Rampton et al. 1984).

As the glaciers retreated from coastal New Brunswick and Maine -13,500 BP the crust remained depressed so that there was a marine transgression that would have created a broad embayment extending inland from the Bay of Fundy (Struiver and Borns 1975;

Rampton and Paradis 1981b; Seaman 1982; Rampton et al. 1984; Shaw et al. 2002). The late glacial marine submergence was termed Lake Acadia by Chalmers (1902) and was believed to be an arm of the Late Glacial De Geer Sea by Kiewiet de Jonge (1951) and

Loughee (1954). However, Seaman (2004) and Foisy and Prichonnet (1991) suggest that

Lake Acadia may have been a later ice-dammed lake due to a Younger Dryas ice readvance from the Caledonia Highlands. Further, Rampton et al. (1984) suggest that the area around the Reversing Falls emerged 12,300 BP and at that time resulted in the dammed Lake Acadia.

The land was initially isostatically depressed under the weight of the ice and, as a result, parts of the New Brunswick Lowlands were submerged to elevations as high as

100 m above present sea-level until approximately 12,700 BP (Rampton and Paradis

1981b; Seaman 1982; Rampton et al. 1984). Others also suggest that maximum submergence occurred between 13,000 and 12,700 BP (Schnitker 1974; Struiver and

26 Borns 1975; Borns and Hughes 1977; Shaw et al. 2002). However, Bloom (1963) suggests that maximum submergence occurred much later, between 12,100 and

11,800 BP. A local sea-level curve for the coastal portion of the State of Maine indicates sea-level rose to a highstand of 70 m, at approximately 15,000 BP (Belknap et al. 2005)

(Figure 1.5).

Sea-level began to fall -15,000 BP at rates up to 43 mm/yr until it reached a lowstand in Maine -12,000 BP of-60 m below present sea-level (Belknap et al. 2005) and -65 m along the Atlantic Coast (Stea et al. 1994). The Bay of Fundy sea-level lowstand occurred -7000 BP (Fader et al. 1977). Shaw et al. (2002) note that Lewis et al.

(1995) used radiocarbon dates from the Grand Banks to determine an initial relative sea- level (rsl) low stand of -100 m -18,000 BP with rsl possibly reaching -125 m. The upper portion of the Saint John River was slower to rebound and remained isostatically depressed; therefore, for a period of time the river drained north into the St. Lawrence

River (Kite 1982, p. 9). However, later isostatic rebound of the upper portion of the river, and the following rise in sea-level, have helped to form the present southerly drainage system.

Following this maximum lowstand, sea-level began to rise again as the rate of isostatic rebound slowed. Relative sea-level for coastal Maine rose at rates up to

22 mm/yr reaching a local sea-level of-20 m at about 9000 BP; rates then slowed again until about 6000 BP (Belknap et al. 2005). Relative sea-level for New Brunswick was also continuing to rise, and sometime between 8000 and 5000 BP the shoreline reached a lowstand of-12 m (Grant 1980). Grant (1970) suggested that until approximately 5000

BP, when sea-level was close to its present position, the Gulf of Maine was largely a

27 30

a Marine Shells 40 D Other lowstand • Salt Marsh Peat ---50 A Marine Shells o Other lowstand -•-60 1 LOWSTAND: ! • Salt Marsh Peat -70 18000 16000 14000 12000 10000 8000 6000 4000 2000 CALENDAR YEARS BP Figure 1.5: Maine, USA, Quaternary relative sea-level data (after Belknap et al. 2005).

28 tideless sea. Evidence for this from the Casco Bay region and adjacent areas of southwest Maine and coastal New Hampshire comes from basal peat dates of salt marshes (Keene 1971; Nelson and Fink 1978), buried shells (Fink 1977) and drowned intertidal to subtidal tree stumps (Hussey 1959).

Tidal range has changed as sea-level has risen along the shores of the Bay of

Fundy. Schnitker and Jorgensen (1990) determined that sometime after 6000 BP modern day diatom flora and foraminiferal faunas were just starting to became established in the

Gulf of Maine; however, the Bay of Fundy region was still primarily a shallow tideless body of water that would not have been highly productive with regard to habitat for clams and anadgemous fish.

Sea surface temperatures started to decline beginning around 4000 BP, and oceanic temperatures became colder in the region (Andrews 1972; Fillon 1976). There was a local extinction of swordfish (Sanger 1975), oysters (Crassotrea virginica), quahogs {Mercenaria mercenaria) and bay scallops (Pecten irridiens), species that are presently found only in warmer waters south of Cape Cod (Yesner 1984). Swordfish numbers declined significantly, as prior to 3500 BP they are represented in abundance in the archaeological record (Sanger and Belknap 1987). Oysters {Crassotrea virginica) and quahogs {Mercenaria mercenaria) can also be found in prehistoric shell middens just west of New Brunswick in estuaries such as the Damariscotta River, Maine (Snow 1972).

These shellfish do not live in the presently colder Damariscotta River area. Sometime between 6000 and 5000 BP water started to flow into the Bay of Fundy, over top of the

Scotian shelf and tides in the Bay began to increase (Scott and Greenberg 1983). Gehrels

(1999) determined that sea-level rise was at 0.75 mm/yr between 6000 and 1500 BP, with

29 an increase of 0.43 mm/yr over the past 1500 years. He further determined that sea-level was fairly stable between 1100 and 400 BP, and only rising 0.5 m during the past 300 years (Gehrels 1999). However, Grant (1970) suggests that sea-level change for New

Brunswick was at approximately 30 cm/century for at least the last 4000 years.

Additionally, high-tide level in the Bay of Fundy has risen at a rate exceeding 2 mm/yr over the last 4000 years (Dalrymple et al. 1990), with modern sea-level rise for the coast of Maine indicating an average rate of sea-level rise of 0.5 to 0.9 mm/year during the past

2500 years (Gehrels et al. 1996).

Water level in the lower Saint John River valley has fluctuated at different times and for different reasons since the end of the last glaciation. Eustatic sea-level rise, local tectonic events, isostatic adjustment and the relaxation of the forebulge, and higher tidal rise have affected the marine limit throughout the Bay of Fundy (Gehrels et al. 1996) and subsequently the lower Saint John River. Additionally, similar events have also been noted to the west in the Penobscot region of Maine (Barnhardt et al. 1995; Kelley and

Sanger 2003). Throughout the Holocene a changing marine limit would have led to a very dynamic environment along the New Brunswick coast, connecting lowlands and tributaries.

Coastal and estuarine valley evolution is strongly related to relative sea-level.

There is no one formula that may be applied to all coastal localities that would unravel relative sea-level change. The level of the sea or of the adjacent land can be different depending on the natural geological processes of a given region (Grant 1970; Scott and

Medioli 1980; Grant 1994; Barnhardt et al. 1995). Ancient sea-levels are often marked by relict beaches, eroded terraces and by glaciomarine deltas (Rampton et al. 1984).

30 Chronological control for these features are often based on local shell dates (Lowdon et al. 1970, 1971; Stea et al. 1994).

Deltas can be found around such features as lakes or sea coasts. The energy level along sea coastlines is considered high, whereas the energy level along lakes is considered lower, but efficient enough for sediment to accumulate given the appropriate environmental conditions. The linear arrangements of the various types of deposited sediments or facies found along lake or sea coasts represents the depositional microenvironments that record the events that occurred upon deposition (Butzer 1982).

However, such depositional features as beaches are not common features associated with the De Geer Sea in New Brunswick (Kiewiet de Jonge 1951), and may be associated with unstable water levels in the early lower Saint John River valley (Rampton et al. 1984).

Watters et al. (1992) suggest that the recognition of ancient shorelines is an important portion of any environmental interpretation pertaining to archaeological site locations. Therefore, it is important to consider the cause and rate of change related to the position of ancient shorelines. Figure 1.6 represents a satellite image (Government of

Canada 2003) marking the 80 m incursion of early marine water into central New

Brunswick at an elevation consistent with shoreline features found in and around

Fredericton and the Burtts Corner area. A Surfer rendition of the 80 m marine incursion is depicted in Figure 1.7. The image gives a general idea of the extent of the water over the Grand Lake area and where the relic shoreline would be relative to the shores of the lower Saint John River today. The image, however, can only serve as a general approximation of the inland extent of the early marine incursion as it has not been corrected for differences in isostatic rebound.

31 /

# r*ri

J**L&r/ ~

Figure 1.6: Landsat satellite image highlighting the incursion of early marine water (light blue) into central New Brunswick at 80 m, with deltas labelled with a triangle and elevations (modified from Thibault and Seaman 1985). Figure produced by J.S. Jeandron 2007.

32 Meters above sea level

Figure 1.7: Three-dimensional 80 m marine inundation into central New Brunswick. Figure produced by J.S. Jeandron 2007.

33 A geological law proposed in 1894 by Johannes Walther may be used as a tool not only in geology but also in archaeological predictive modeling. Walther's Law states that facies originally horizontally adjacent to one another will be found in strati graphic succession, with the vertical facies mirroring the horizontal facies. It should be noted that gaps, leaving an incomplete shoreline sequence (Prothero and Schwab 1996), could be formed within shoreline sequences or facies due to rapid environmental changes. Such gaps are noted by Rampton et al. (1984) and Kiewiet de Jonge (1951) in the Saint John

River valley. Nevertheless, if it could be predicted where a shoreline occurred at a particular time by using Walther's Law and then develop a geochronology for the successive changes in the shoreline, this would aid in predicting where archaeological sites for particular time periods may have been relative to the present day shoreline.

Prior to the land rebounding, marine deposits have been found that mark the position of the landward extent of the marine invasion in New Brunswick. Early observations by Seaman (1982) suggest that the marine incursion may have reached a maximum of ~90 m, whereas Rampton and Paradis (1981b) suggest it may have reached an even higher elevation at ~120 m. Observations made by Rampton et al. (1984) also place the marine incursion at over 100 m. A number of late glacial features have placed the marine incursion slightly lower, at between 67 and 88 m asl (Matthew 1872;

Chalmers 1885, 1890; Gadd 1973; Grant 1980; Seaman 1982). Observations made by

Goldthwait (1912, 1924) at Saint John and Pennfield puts the marine limit at 68.5 m. On the north bank of the Saint John River from Cullerton to a point opposite Barony Station marine terraces were noted at 88 m (Kiewiet de Jonge 1951).

34 New Horton Lake , along the southeastern coast of New Brunswick, is presently 8 to 10 m above MSL; at this location a date was obtained (8400 BP) that was similar to that found at 49 m above present MSL in southwestern New Brunswick at Bocabek Lake

(Figure 1.8). Scott and Medioli (1980) suggest this may represent the marine maximum in these areas. Slightly inland from Saint John, at West Bay, Chalmers (1890) places marine terraces at 53 to 55 m. Inland at Browns Flats, Kiewiet de Jonge (1951) identified a delta that had an average top elevation of 57 m. Kiewiet de Jonge (1951) also noted deltaic kame terraces with a top elevation of 44 and 63 m in the Nashwaak valley just north of Fredericton. Northwest of Fredericton, in the Mactaquac valley, a delta deposit is located near the junction of the Mactaquac and Little Mactaquac Rivers with an elevation of 59 m (Kiewiet de Jonge 1951).

The elevation of the maximum extent of the marine incursion has been postulated from deltas, marine terraces and beach elevations found throughout the lower Saint John

River valley. These landscape features may be found at lower elevations (i.e. 44 to 63 m) close to the coast and at higher elevations inland (i.e. 67 to 88 m), where ice would have been thicker and therefore where greater rebound may have occurred. This has been suggested by Kite (1982) who has indicated that isostatic depression was greater in the upper portion of the river, where, for a time, water drained north into the St. Lawrence

River. In Maine, glacial-marine deltas also have been identified marking the highstand shoreline. They are currently found at elevations ranging from ~70 m in mid-coastal areas (Dorion et al. 2001; Retelle and Weddle 2001) to at least 128 m in the interior, where ice was thicker and rebound greatest (Thompson et al. 1989). Therefore, observed differences in the elevation of shoreline and/or delta features found throughout the Saint

35 £ V^ Prince Edward Island U.S.A. New Brunswick

New Hon Lake, Bocabec .Lajce

Nova Scotia %

Figure 1.8: New Horton Lake and Bocabec Lake in southern portion of New Brunswick.

36 John River valley can be explained in part by differential isostatic rebound due to ice thickness. However, if a glacial lake subsequently developed in the river valley, some of the shoreline features, such as deltas, may represent a mixture of elevations depicting the later glacial lake, as well as the earlier post-glacial marine inundation. This is noted in the delta elevations found within the lower Saint John River valley (Figure 1.6), which do not show a linear progressive change in elevation depending on distance from the coast.

1.6 Physiography

New Brunswick is the largest and northernmost of Canada's Maritime Provinces.

The province has been divided into six geomorphologic regions (Rampton et al. 1984), which includes the Edmundston Highlands, Chaleur Uplands, Miramichi Highlands, St.

Croix Highlands, Caledonia Highlands and the New Brunswick Lowlands. The Saint

John River has been further divided into three sections denoting differing physiographic and ecological environments (Choate 1973, p. 7), which have been described as:

- the upper Saint John River including the area between the headwaters of the

river to Grand Falls,

the middle Saint John River encompassing the region between Grand Falls

and the head of tide at Mactaquac, and

the lower Saint John River including the area from the head of tide to the

mouth of the river where it empties into the Bay of Fundy.

The Saint John River valley is a major physiographic feature that cuts through the province from north to south. The drainage area for the river encompasses 55,000 km

(Hustins 1974, p. 1), and includes part of Quebec, New Brunswick and the state of Maine

37 (Putnam 1952; Blair 2004). Within New Brunswick the river valley forms a deep trench that cuts through the New Brunswick Uplands, Highlands and Lowlands. The mouth of the Saint John River, as it empties into the Bay of Fundy, divides the St. Croix Highlands, west of the river, and the Caledonian Highlands, east of the river. However, the frequency and magnitude of water and sediment yields transported by the river is not only dependent on physiography, but also climate and vegetative cover (Knox, 1983).

The interior region of the Saint John River valley is deeply penetrated by branching rivers, with the Saint John River being the largest of these river systems. The type of drainage system prevailing in the valley is largely controlled by the surficial deposits, slope, parent material, and underlying structure of the bedrock. Although the

Saint John River, as a whole, is rich in tributary rivers and streams, overall it is poor in large water bodies (Hustins 1974, p. 15).

The lower Saint John River contains eight major tributaries, one salt marsh system, 11 large water bodies, and three major freshwater wetland systems. The current character of the lower Saint John River valley is not indicative of its past. Like many other large rivers it has experienced numerous cycles of channel incision and filling.

Throughout the lower portion of the Saint John River valley there is a series of major landscape zones - higher terraces, lower terraces and active fioodplain. It is likely that elements of each were utilized by people at various times in the past.

1.6.1 Grand Lake Meadows

The Saint John River and adjoining Grand Lake Meadows are subject to tidal influences. The river has an elevated salinity level below the head-of-tide, and includes

38 the lower 140 km of the main river and an additional five large tributary rivers, affecting

. 15,000 km2 of the entire drainage system (www.sararegistry.gc.ca/status/status_e.cfm).

The Grand Lake region contains a large system of open water bodies. Outside of

flood season it contains almost 22,000 ha of open water with swamps and marshes

concentrated in several areas (Dzikowski et al. 1984; NBDNRE 1998). The largest of

these are the Grand Lake Meadows, which provide a complex setting for migrating

waterfowl, aquatic and terrestrial plants and animals, and unique associations of

hardwood swamp vegetation (Choate 1973). The total region of the Grand Lake

Meadows consists primarily of a broad flat floodplain and wetland meadow, with

topographic relief ranging from just above sea-level to an elevation around 40 m. The

higher relief represents bedrock hills and knobs, around which the Grand Lake Meadows

lower flat lands were deposited.

The land encompassed by the Grand Lake Meadows was classified by Washburn

and Gillis (1996: 2-1) as Floodplain Wetlands. This was because on any given year,

approximately 85% of the area is inundated by seasonal floodwaters. The Flood Risk

Map (NBDOE 1981) for Oromocto and Lower Jemseg shows that the 1973 spring flood

inundated the whole of the Grand Lake Meadows, as the high water level reached 8.54 m

at Fredericton. The susceptibility of the Grand Lake Meadows to flooding is a function

of the low topographic relief of the area coupled with the fact that the constricted nature

of the gorge at Reversing Falls in Saint John, only allows for a limited amount of outflow

of water per week, regardless of the tides and season (SJRBB 1972). This constricted

nature of the gorge results in the periodic accumulation of large volumes of water during

times of high river flow that causes flooding upriver. This flooding happens annually

39 after snowmelt in the spring and causes large volumes of sediment to be deposited in the

Grand Lake Meadows area. This is one of the primary factors leading to the formation of the bottomlands of the lower Saint John River region.

1.6.2 Major Geomorphological Events

At the mouth of the Saint John River, where it flows into the Bay of Fundy, tidal inflow and outflow of the river has led to the estuarine environment found within the lower reaches of the river today. This postglacial exit of the river over the Reversing

Falls is not the preglacial outlet for the Saint John River. Chalmers (1885, 1890) and

Matthew (1894) proposed that a buried preglacial outlet channel existed for the Saint

John River at Saint John West. Later, a seismic survey of the area by Hawkins (1978) delineated a wide, deep preglacial river channel that was cut into the bedrock from South

Bay across Churchill Heights and Island View Heights to the Bay of Fundy coast. This outlet was later filled with post-glacial moraine deposits (Manawagonish Moraine) damming the preglacial exit of the Saint John River (Gadd 1973). Water eventually cut a path through the bedrock obstruction at the Reversing Falls and a new outlet for the Saint

John River developed. Water depths reach 30 to 42 m at the entrance to the Falls section, but only a depth of between 0.9 and 7.6 m over the sill at low-tide (Flaherty 1989, p. 10).

Two of the major geomorphological events that have affected the lower Saint

John River basin during the late Pleistocene/early Holocene include the formation and draining of a glacial lake and the formation of an estuary. Along with these geomorphological events were climatic shifts and changing patterns of local and regional vegetation, all of which would have impacted human occupation within the region.

40 1.6.2.1 Formation of a Glacial Lake

At some time during the Holocene a barrier at the mouth of the Saint John River permitted the development of an inland river and lake system, which occupied a significant portion of the valley bottom. This barrier was ultimately breached and the subsequent inland river and lake system began to drain. Such an event would result in a significant and immediate change in watercourse dynamics within the lower portion of the river, both affecting the environment and early human occupation.

Matthew (1894) suggested that after the land had been depressed by the weight of the ice and was submerged under the sea it began a slow rise so that early elevated ridges, such as found at the site of the Reversing Falls (Rampton et al. 1984) emerged forming a barrier between the coast and the lower Saint John River valley. Gadd (1973) suggested that there was a significant halt to the retreating ice margin contributing to the creation of an ice-dammed lake in the lower Saint John River valley halfway between the Bay of

Fundy and Fredericton. Seaman (2006) and Foisy and Prichonnet (1991) later postulated that an active ice cap present in the Caledonian Highlands may have expanded northward onto the adjacent New Brunswick Lowlands and across the lower Saint John River valley serving as a dam and holding a large amount of water within the lower portion of the valley.

Previous to the formation of the Glacial Lake, the entire sediment load carried by the main river channel would have been delivered to the sea. However, once this glacial lake came into existence, and if it was stable for any length of time, it would have functioned as an efficient sediment trap, building up a number of beach terraces around its perimeter. However, such features are limited in the lower Saint John River valley

41 (Kiewiet de Jonge 1951; Rampton et al. 1984). Today a few concentric beach ridges are present following a north/south transect through the lower Saint John River valley

(Kiewiet de Jonge 1951). However, these beach ridges can also be associated with uplift, possibly relating to early tectonic activity in the region and the subsequent inland sea.

Rampton et al. (1984) suggest that the glacial lake occupied the lower Saint John River valley during the Madawaska phase of the late Wisconsinan (~12,000 BP). The formation of this lake would have been a critical event in the formation of the early environment and landscape in the region.

1.6.2.2 Formation of an Estuary

The mouth of the Saint John River is constricted by what is today called the

Reversing Falls gorge. Approximately 10,000 to 8000 BP, when the mean sea-level of the Bay of Fundy was as much as 60 to 85 m lower than at present (Grant 1970; Gadd

1973; Amos et al. 1980; Rampton et al. 1984; Kellogg 1988) the river flowed over a bedrock sill into what is today the Bay of Fundy. Flaherty (1989) notes that using geophysics and continuous depth sounding of the Reversing Falls, two post glacial waterfalls were found at the current outlet of the Saint John River. These waterfalls would have acted as plunge pool basins when sea-level was lower. The upriver waterfall formed a 45.7 m deep basin, with the lower waterfall reaching a depth of 51.8 m

(Flaherty 1989).

It has been determined that about 6000 BP water started to flow into the Bay of

Fundy, over top of the Scotian shelf (Scott and Greenberg 1983). At this time these waterfalls would have been continually draining the Saint John River. Rampton et al.

42 (1984) suggest that a slow submergence of the Bay of Fundy coast has been occurring for the last 4000 years. From this Flaherty (1989) argues that 4000 years ago these early waterfalls were inundated by water from the Bay, reversing flow over the falls at high tide.

When the Saint John River flowed over the sill at Reversing Falls into the Bay, the river would have been an exclusively freshwater system. During the early to mid-

Holocene, the waterfall at the mouth of the river was transgressed by marine waters from the Bay of Fundy during high tide, flowing up-river into the lower portion of the Saint

John River creating the modern estuary. The saline character of the lower portion of the

Saint John River is not new. Postglaciation, the Saint John River valley was flooded with saline water from the early inland sea, after which time emergence of the Reversing Falls area above relative sea-level, temporarily ended this direct connection with the Bay of

Fundy (Rampton et al. 1984).

1.7 Previous Core Analysis in the Fredericton Area

Previous research in the Fredericton area (borehole UNB-1-03 and Waasis borehole BH-1) (Daigle 2005) and the Fredericton Junction area (Giudice 2005) indicates that the nature and extent of geological events post glaciation were somewhat different in these two locations. ICP-OES results were conducted for chloride on sediment from both . locations (Giudice 2005). Results from the Fredericton data set indicate that there was a low concentration of chloride present suggesting deposition may have occurred under brackish water conditions. Similar analysis was completed on the sediment from the

Fredericton Junction core and indicated that no chloride was present.

43 XRD results from the City of Fredericton and Fredericton Junction data set indicate that quartz, clinochlore, muscovite and albite mineralogical compositions are similar within the two areas, whereas calcite was absent from the Fredericton Junction data set. The sediment sources for the two areas are thought to be the same. Therefore

Guidice (2005) suggests that the calcite found in the Fredericton data set may represent a marine or brackish water depositional environment, whereas the lack of calcite in the

Fredericton Junction sediment represents freshwater glaciolacustrine deposition.

Geotechnical analysis that included atterberg limit tests to determine the liquid and plastic limits of the sediment, determined that the Fredericton Junction data set has lower clay content than the Fredericton data set. Additionally, particle size analyses revealed that the Fredericton Junction sediments are siltier than those from Fredericton and more representative of a clayey-silt rather than clay. Guidice (2005) suggested that this difference in sediment reflects proximity to the ice and sediment source during the time of deposition. The clayey-silt in the Fredericton Junction data set represents close proximity of the ice or the tributary did not undergo marine submergence, whereas the clay from the Fredericton core is representative of a marine environment probably located some distance from the ice front (Guidice 2005).

Results from the Fredericton (Daigle 2005) and Fredericton Junction (Guidice

2005) studies indicate that the Fredericton Junction area did not experience an inundation of marine water post glaciation, whereas the data set from Fredericton indicates evidence for marine deposition. This is suggestive that there were limits to the marine incursion into the tributaries of the Saint John River.

44 CHAPTER 2

ARCHAEOLOGY OF THE LOWER SAINT JOHN RIVER VALLEY

Since the 1970s a number of archaeological research programs have focused on a series of prehistoric sites in the New Brunswick portion of the Saint John River (Sanger

1971a, 1971b, 1973, 1991; Allen 1975; Turnbull 1975,1990; Burley 1976; Ferguson

1983; Keenlyside 1992, 1993; Keenlyside and Allen 1993; Black and Wilson 1999;

Bourgeois 1999; Dickinson 2001; Blair 2004). However, little research has focused on the geomorphological landscape surrounding these sites. Aside from research being completed at the University of New Brunswick, as part of the Masters program in archaeology (MacDonald 1994; Blair 1997; Bourgeois 1999; Suttie 2005), most archaeological projects focusing on the lower Saint John River valley has been guided by government agencies and consulting firms with the aim of recording and maintaining preliminary site inventories and determining the archaeological potential of particular locations prior to construction. Such research has included a number of major excavations of pre-contact sites related to highway development within the lower Saint

John River valley (Blair 1997; Washburn and Gillis Associates 2000; JWEL 2003, 2004).

However, this lowland river landscape has been relatively undisturbed due to the subsequent alluviation leading to the creation of buried and sometimes still waterlogged landscapes, and the presence of elevated terrace gravels.

45 2.1 Culture History

Archaeologists have attempted to develop a regional chronological framework for the distribution of cultural material. This chronology has recently been further delineated for the lower Saint John River valley (Blair 2004). The archaeological culture periods for

New Brunswick are divided into four time periods, the Palaeoindian, Archaic, Maritime

Woodland and Historic, which are based primarily on the material remains that were left behind.

The following brief summary of the archaeological sequence for New Brunswick illustrates the record of First Nations use of this area and the region's culture history.

Research driven from both academics and consultants continues to refine the culture history of New Brunswick and introduces new information that may change current ideas. Although dates are given for each culture period, these are only general guidelines that relate to periods that have specific defining characteristics.

2.1.1 Palaeoindian Period (prior to 9000 BP)

During the Wisconsinan glaciation, which lasted from approximately 25,000 to

14,000 BP, most of the Maritimes region was covered by a thick mantle of ice, which probably exceeded several kilometers in thickness. The first people into the region after the glacial ice started to retreat were living on a dynamic landscape and are known as

Palaeoindians.

The Palaeoindian culture period is not well represented in the prehistoric chronological sequence for the Maritime Provinces; it is divided into an Early (up to

10,000 BP) and Late (10,000 to 9000 BP) Palaeoindian culture period. Not being well

46 represented in the Maritime Provinces, and in particular New Brunswick, may be the result of several factors, such as the submergence of sites by a rising sea-level, site locations not consistent with those of later periods, or the small number of researchers working in this area. However, an understanding of the Palaeoindian cultural traditions has grown significantly in recent years as a result of Palaeoindian sites that have been identified in the neighbouring state of Maine and provinces of Nova Scotia, Prince

Edward Island and Quebec (MacDonald 1968; Gramly 1982; Keenlyside 1985; Spiess and Wilson 1987; Davis 1991; Chapdelaine and Bourget 1992; MacCarthy 2003). There have been no identified archaeological sites that date to this early culture period within the province of New Brunswick; however, there have been six isolated Palaeoindian projectile points found within the province (Turnbull 1974; Turnbull and Allen 1978;

Dickinson and Jeandron 1999). Additionally, the Jemseg Crossing site (BkDm-14) produced artifacts that may also be indicative of the Palaeoindian period (Dickinson

2001).

There have been a number of settlement and subsistence models postulated for

Palaeoindian people in the Northeast. Many of these models suggest that Palaeoindian sites in this region exhibited considerable diversity, ranging from small scouting party sites to large habitation sites, kill sites and quarry sites (Loring 1980; MacDonald 1982;

Storck 1984, 1993; Bonnichsen et al. 1985, 1991; Gramly and Funk 1990; Ellis and

Deller 1997; Tankersley et al. 1997; Spiess et al. 1998). Information obtained from palaeoenvironmental data, combined with what is currently known of Palaeoindian site locations, suggest that the arrival of Palaeoindian people into the region may be linked to the Younger Dryas period, suggesting these early inhabitants may have lived in an ice

47 marginal environment (Davis and Jacobson, Jr. 1985; Hughes 1987; Joyce 1988; Kite and

Stuckenrath 1989; Cwynar et al. 1994; Jones 1994). It has been postulated that the timing of Palaeoindian people in the region is also linked with the timing of the postglacial DeGeer Sea (Loring 1980; Dincauze and Jacobson 2001). Additionally, a number of Palaeoindian sites from Maine and Ontario have been found in association with the strandline of early glacial lakes (Storck 1984; Bonnichsen et al. 1991) suggesting that site preference may have been along lakes, rivers, ponds or bog edges (Storck 1984).

Sites from Maine, Nova Scotia and Quebec have been located on glacial features such as outwash deltas, kame terraces and marine terraces, locations having relatively dry, level and well-drained expanses of sandy soil (MacDonald 1968; Gramly 1982; Spiess and

Wilson 1987; Bonnichsen et al. 1991; Chapdelaine and Bourget 1992). Artifacts diagnostic of the Palaeoindian period consist of Clovis and Piano style projectile points.

It is also possible that the presence of a longitudinal flake down the center of the spur on a spurred end scraper may also be diagnostic of the Early Palaeoindian period (Dickinson

2001).

2.1.2 Archaic Period (9000 to 2800 BP)

The Archaic period is further divided into a number of sub-periods in the archaeological literature. The Early Archaic (9000 to 7000 BP) and the Middle Archaic

(7000 to 5000 BP) are periods which archaeologists are only beginning to comprehend in the Maritimes, whereas archaeologists have a better understanding of the Late Archaic

(5000 to 3600 BP) and Terminal Archaic (3600 to 2800 BP) periods. Also, regional diversity of artifact types has been sorted into several phases, complexes and traditions.

48 These include the Vergennes phase, from -5200 to 5000 BP (Funk 1988; Cox and

Wilson 1991; Tuck 1991; Robinson 1996), the Small-Stemmed Point tradition, from

-5200 to 4200 BP, (Tuck 1991; Bourque 1995; Petersen 1995; Robinson 1996) the

Moorehead phase, -4400 to 3800 BP (Sanger 1973, 1991; Tuck 1991; Robinson 1992;

Bourque 1995), and the Susquehanna tradition, from -3800 to 3500 BP (Tuck 1991;

Bourque 1995; Robinson 1996).

It has been hypothesised that there is an apparent gap in the archaeological record between 10,000 and 5000 BP, which has been referred to as the "Great Hiatus" by Tuck

(1984). Fitting (1968) suggests that there was an unproductive environment at this time, which was in turn responsible for a low population density. However, archaeological information from New Brunswick, Maine and Newfoundland that contributed to the

Archaic period and brought the "Great Hiatus" hypothesis into question includes excavated sites of an early Holocene age, reanalysis of existing collections, and numerous radiocarbon dates that range between 10,000 and 5000 BP (Robinson 1992, 1996; Blair

2003, 2004). Petersen (1995), Murphy (1998), Suttie (2007) and Deal et al. (2006) assisted in the development of a new model for Early and Middle Archaic occupation that negated the hypothesis of a "Great Hiatus".

Evidence for Early and Middle Archaic sites in New Brunswick has been identified primarily from artifacts recovered from private collectors (Murphy 1998). The

Jemseg Crossing site (BkDm-14) produced artifacts that may be indicative of the Early or

Middle Archaic period (Blair 2003), as did sites located within the Lake Utopia area, northwest of Passamaquoddy Bay (Suttie 2005). Also, there have been numerous surface collections from within the lower Saint John River valley that contain artifacts considered

49 diagnostic of the Middle Archaic and earlier (Sanger 1973; Murphy 1998), such as fully grooved gouges, ground stone rods and semi-lunar knives. A number of stone tools representative of this period have been found offshore, pulled up by scallop draggers

(Black 1996), possibly suggesting a lower sea-level during this period. Such finds work well with the hypothesis proposed by Sanger (1975, 1979) and Tuck (1991) suggesting that the low number of Early and Middle Archaic sites may relate to sea-level changes along the Atlantic shores. It has been postulated that the vast majority of Early and

Middle Archaic sites along the coast or within the associated estuaries may now be submerged (Murphy 1998, p. 88). Also, a number of well-stratified early Holocene sites have survived in deeply buried riverine alluvium (Petersen and Putnam 1992; Murphy

1998). Murphy (1998) suggests that river channels that are not stable may meander and bury cultural material at locations away from modern river channels, or alternatively, erode them altogether. This fact along with the lack of projectile points from Early and

Middle Archaic sites (Sanger 1996) may impede identification of such early sites.

There is a much better understanding of the Late Archaic period as many more sites from this time have been identified in New Brunswick. Some Late Archaic sites are easily recognized by the use of ground haematite (i.e. the Cow Point site from the Grand

Lake region, Sanger 1973, 1991). The ground haematite was often used in ceremonies that included burials. Artifacts associated with this period often included ground slate bayonets and semi-lunar knives, fully and partially-channeled gouges, ground stone rods, plummets, celts and assorted projectile point types. It was also during the end of this period that the use of pottery was established in the region. Originally imported bowls

50 carved from steatite were introduced and later a clay fired ceramic technology was adopted.

2.1.3 Maritime Woodland Period (2800 to 500 BP)

As with the previous cultural periods, the Maritime Woodland is broken up into three sub-periods, Early, Middle and Late. The Early Maritime Woodland Period (3000 to 2150 BP) begins with the introduction of undecorated pottery into the archaeological record, and a change in projectile point style from those that have a straight stem to those that are side notched. Native people began making ceramic pottery containers to serve a variety of cooking and storage functions. Also, aboriginal groups were acquiring small amounts of native copper and making finished copper items that included rolled copper beads that were used for decoration and traded (Rutherford 1990).

Two cultural manifestations are known for the Early Maritime Woodland, the

Meadowood and Middlesex or Adena (Rutherford 1990, 1991). Early Maritime

Woodland Period sites are generally thought to be riverine oriented and tend to be either ceremonial or habitational. Artifacts associated with such sites often include celts, pottery, box-based side-notched projectile points and atl-atl weights. Such sites have been found in the Jemseg area of the lower Saint John River valley.

The Middle (2000 to 1400 BP) and Late Maritime Woodland Period (1400 to 500

BP) designations are based primarily on differences in ceramic style and decoration. The ceramic manufacturing process differs chronologically and geographically by design, vessel size, wall thickness and foreign inclusions (Foulkes 1981; Petersen and Sanger

1991; Bourgeois 1999). Earlier ceramic designs include pseudo-scollop shell and rocker

51 dentate patterns. Later Maritime Woodland Period ceramic decoration included cord- wrapped stick, linear incising and circular punctuates. There also seems to have been a change at approximately 650 BP from the use of conical-based ceramic vessels to ones more globular shaped. During the Middle and Late Maritime Woodland Periods local copper was also collected and made into usable tool forms (Leonard 1996).

Aside from differences in ceramic style and manufacture it is difficult to distinguish between Middle and Late occupations at most archaeological sites. The

Middle Maritime Woodland Period sites are commonly found along the banks of the

Miramichi River, Bay of Chaleur and Grand Lake, with later Maritime Woodland Period sites found along the Fundy coast. The Maritime Woodland Period ends at the time of

European contact (-500 BP).

2.2 Archaeology of the Grand Lake Meadows

Archaeological sites are any place where artifacts or cultural features are found, and can range from "find spots" of individual artifacts to large habitation sites or cemeteries. Archaeological sites are registered with the province in the New Brunswick

Archaeological Sites Database. When a site is registered relevant information regarding the site such as content, structure and location is recorded, and it is then placed within the nation-wide borden system. The borden system is a geographically based method for recording archaeological sites. In New Brunswick, each borden block is 10 minutes of latitude by 10 minutes of longitude. Each of these blocks is referred to by a four-letter code that corresponds to the location of the archaeological site.

52 Within the lower Saint John River valley, only 18 of the known precontact sites have produced artifacts or features from an excavated context (Blair 2004, p. 177). Table

2.1 lists the precontact sites identified within the Grand Lake Meadows area. Of these sites only the Fulton Island site, BlDn-12 (Foulkes 1981) and The Meadows site, BlDn-

26 (JWEL 2004) have been excavated. All eight sites identified within the Grand Lake

Meadows date to the Woodland cultural period (2800 to 500 BP). Two sites just outside the Grand Lake Meadows area date to the Late Archaic (5000 to 2800 BP). The

MacKinnon-Jemseg River site, BkDm-14 (Blair 2004), is located on the east bank of the

Jemseg River and the Cow Point site, BlDn-2 (Sanger 1973), is located on the southwestern bank of the Saint John River.

Borden # Site Name BlDn-3 Jemseg River BIDn -8 Ring Island BlDn-12 Fulton Island BIDn-18 Interlake BIDn-19 No name given BIDn-21 No name given BIDn -23 No name given BIDn -26 Meadows Table 2.1: Precontact archaeological sites identified within the Grand Lake Meadows.

2.3 Spoken History of the Lower Saint John River Valley

In historic times the Saint John drainage, along with the Tobique and Temiscouta areas, up to the St. Lawrence River, were major portions of the Wolastoqiyik (Maliseet) territory. Therefore, the Wolastoqiyik have a strong tie to the Wolastoq (Saint John

River) and have a unique connection with the landscape. This connection resides in the memories of the Wolastoqiyik.

53 The spoken histories of New Brunswick Aboriginal People can provide information on the character and history of a particular landscape or the perceptions of a landscape by the People. Often the dominance of nature and the significance of rivers and lakes within their lives can be seen in these stories. Information within spoken histories, for example, can help to clarify the connection of the Wolastoqiyik within the

Saint John River valley (Blair 2003), ancestral Wolastoqiyik territory (Ganong 1899,

1904; Deal 2002). Wolastoqiyik have always lived, traveled, traded, hunted, gathered and fished throughout the Saint John River drainage basin. Through some of the spoken histories of the Wolastoqiyik it is possible to glimpse how their surroundings, such as the

Saint John River itself, changed through time. This is an account written by Webster

(1930) that talks about the modern falls at the mouth of the Saint John River:

These have attracted great attention since the white man first came to the province and they have been described by Champlain, Lescarbot, Denys and many other explorers and writers. The peculiarity of the falls is that they reverse; part of the time the water rushes upwards, and part downwards. Where they are situated, the river narrows to a width of 350 feet, the limestone banks being walls nearly 100 feet high, and the bed of the river consists of sharp rocky ledges. At low tide a mighty volume of water rushes downwards over these forming a turbulent rapid. As the tide again rises (Saint John Harbor tides may reach nearly thirty feet) it meets the river current at the falls, over-comes it and rushes upwards over the falls with great velocity. This struggle takes place twice in every twenty- four hours (Webster 1930, p. 43).

Webster (1930) also writes about what he calls the Indian legend of the origin of the falls:

Glooscap, ever watchful over the interests of the Indians, controlling the forces of nature as well as all the animals, was informed that the Big Beaver was annoying some of the other animals, and he, there-upon, cautioned him as to his future conduct. However, the beaver continued to misbehave in the Passamaquoddy district and Glooscap went after him. Big Beaver, learning of this, fled to the mouth of the river Saint John (Men-ah-questk) and built a dam

54 across it so high that the whole country was flooded above it for many miles forming a Jim-quispam or huge lake. Glooscap scoured the country in search of the beaver but did not find him. When he arrived at Saint John and saw the dam he smote it with his mighty club breaking it, so that the great rush of water carried a piece of it outside the harbor, where it became deposited forming an island (now called Partridge Island). The great lake which existed above the dam was reduced, a much smaller area being left as the present Grand Lake. The split-rock seen below the falls was believed by the Indians to be Glooscap's club, which he threw there after smashing the dam. The Indian name of the falls means "the beaver's rolling dam". It may interest the curious to know that Glooscap finally found and killed Big Beaver (Webster 1930, pp. 43-44).

The Mi'kmaq also have flood stories. This is an account written by Norman

(1990) and Leland (1992) that talks about Ice Giants and rushing water:

Kuloscap (Glooscap) defeated the cruel Ice Giant magicians at various contests. Then he stomped on the ground, and foaming water rushed down from the mountains. He sang a song, which changed how everyone looks, and the Ice Giants became large fish and were washed to sea. Those fish carry markings like the wampum collars of the magicians (Norman 1990, p. 115; Leland 1992, p. 126).

It is interesting to see how the geological reconstruction models for the lower

Saint John River valley complement the First Nations' spoken histories for the region.

Each Native language group documented, through their spoken histories, particular aspects of the landscape and landscape change that geologists have only recently begun to understand.

55 CHAPTER 3

INVESTIGATION METHODS

Interest in palaeoenvironmental analysis is growing, particularly along coasts and estuaries, due to an increased awareness of climate change and the desire to forecast more accurate future conditions. Palaeoclimatic records obtained from the analysis of a continuous sediment core extracted from surface to bedrock within the Grand Lake

Meadows can allow for a more inclusive analysis of climate and landscape change for this region.

Sediment cores can help to infer regional climatology and ecology. When deep sediment sequences are dated reliably using radiocarbon or other methods the timing of past environmental changes can be estimated. Continuous sediment records obtained from the GLM-01 core documents the late Pleistocene and Holocene landscape for the

Grand Lake Meadows region.

3.1 Drilling and Coring

The floodplain and alluvial setting of the lower Saint John River valley is today and has been in the past a dynamic environment for human habitation. People persisted and still persist in living and working in an area that is subject to sometimes hazardous events, such as flooding and soil erosion. Therefore, a consideration of the positive and negative significance of past geological factors that would have impacted the landscape is important in gaining an understanding of where to obtain a sediment core. This would allow for the retrieval of a high quality sedimentary sequence that would be

56 representative of the general sedimentation pattern for the region. The balance between a stable and unstable landscape will change over time, as a result of geological and climatological change.

The dynamic environment of a floodplain, such as can be found in the lower Saint

John River valley, can lead to difficulty in developing landscape models. Depositional sequences may preserve past landscapes but also render them invisible, whereas erosion sequences, such as the wearing away and movement of earth material by gravity, wind, water and ice may leave little to no trace of similar landscapes. Brown (1987) draws attention to the lack of mobility of many lowland rivers often caused by resistant banks formed by cohesive sediments and/or low stream power resulting from low regional slopes. The lower Saint John River has been a meandering system throughout the

Holocene, as revealed in aerial photographs from the region depicting old channels, meander belts and oxbow lakes (Figure 3.1). Therefore, it was important to choose a drilling location for the GLM-01 sediment core that was in the past, and is today, a stable landscape feature.

The setting of the extracted sediment core is within Queens County, the Parish of

Canning, along highway 105 (Figures 1.2 and 3.1). Coordinates for this location are'45°

50' 14" latitude and -66° 10' 33" longitude (NAD830CSRS). The site is situated on an elevated channel bar located between the current Saint John River and Grand Lake.

Grand Lake is 2 m above sea-level even though it is more than 70 km from the open marine waters of the Bay of Fundy. The location where the core was extracted exhibits wide, valley topography and is at an elevation of approximately 4.144 m above mean sea-

57 .1: Areal photograph with drilling location marked (Service New Brunswick orthophotoniap, Grand Lake, map sheet 45806610, 01/02). level. The site area is ploughed and is currently being used for agriculture purposes

(Plate 3.1).

The location of the GLM-01 core was based on criteria that indicated a dry stable landform. It was important to place the GLM-01 core close to the center of the palaeochannel so as to obtain the deepest continuous sediment core possible from the region. Additionally, since the Grand Lake Meadows is the largest wetland complex in

New Brunswick it was important for drilling to place the core within the driest part of the meadows region. The drilling was on an aggrading channel bar sequence, which frequently during the spring becomes gradually flooded and buried by overbank sediments producing a stable sealed land surface.

To maximize the amount of information obtained from the sediment core it was important to place the core in a location that has been stable and undergone the least amount of erosion. With Holocene floodplain aggradation in the region, channel bars frequently become gradually flooded and buried by overbank sediments producing sealed land-surfaces that undergo relatively little surface erosion. It was important that the drilling site be situated in a location that would allow for the deepest sediment core possible to be extracted from the basin.

RockWorks 2002 software was used to create a cross-section for the Grand Lake

Meadows region to enable stratigraphy and depth to bedrock to be determined across the river valley and help pinpoint a location for drilling. The borehole records used for the analysis came from consulting reports and government documents. The RockWare

59 Plate 3.1: Drill at core location within the Grand Lake Meadows (photo by P. Dickinson).

60 software allowed the author to develop a stratigraphic model across the two major rivers within the Grand Lake Meadows; the Saint John River to the west of the Meadows and the Jemseg River to the east, as well as indicated that the Grand Lake Meadows is located within the center of a large palaeochannel (Figure 3.2). Each borehole record, including coordinate, elevation and total depth was entered into a project database using

RockWorks 2002. Descriptive lithologies for each unit, including corresponding depths, were also entered into the database. The data were standardized to a common system of metric units and all coordinate data were converted to New Brunswick Double

Stereographic NAD 83 Zone 19 UTM Northings and Eastings. Borehole record information was first described by lithology and then assigned a lithostratigraphic unit.

Depth to the top of each lithologic layer was converted to metric units above mean sea- level. The interpretive stratigraphy was then assigned based on the sequence in which the lithostratigraphic units appeared. The interpretive stratigraphy was based on the conceptual model of deposition relative to glaciation and post-glacial events. Each individual borehole was then examined in relation to the neighbouring boreholes which facilitated the development of the cross-sections. Once the cross-sections were made for each river system, they were verified against one another. Additional discussion of these procedures can be found in the RockWorks 2002 user manual.

The primary fieldwork for this project took place over a five day period, from

June 14 to 18, 2006, and consisted of a continuous sediment core drilling project. A total of 67.51 m of sediment core was recovered from the GLM-01 core. The methodology included drilling a 7.5 cm diameter borehole from surface to bedrock. A continuous coring technique was used employing 75 cm long, 7.5 cm diameter Shelby tubes, and

61 Figure 3.2: Stratigraphic model across the two major rivers within the Grand Lake Meadows; the Saint John River (a) to the west of the drill location and the Jemseg River (b) to the east. Drill hole locations marked with a triangle and line. The colour code highlights the modern river (dark blue), modern fluvial (light blue), fluvial (orange), lower ponded environment (grey/blue), early lower ponded environment (red), till (green) and bedrock (pink).

62 60 cm long, 3.5 cm diameter Split Spoon samples, as it allowed for the stratigraphic integrity of the deposits to be conserved. The method of continuous coring allowed for- uninterrupted and direct observations to be made of the sedimentary context of the samples.

After obtaining landowner permission and acquiring a Scientific Protected

Natural Areas Permit from the Department of Natural Resources, Lantech Drilling

Services Inc. of Dieppe, New Brunswick, started the drilling project using a track mounted hollow stem auger drill rig (Plate 3.2). Core samples were collected along the full depth of the loose unconsolidated soils to till using split spoon samplers (Plate 3.3).

For the more cohesive soils Shelby tubes were utilized (Plate 3.4). Core samples were collected every 0.6 m for the top 30 m of the hole and every 0.8 m for the remaining 30 m of the hole. Till was encountered at 60.5 m depth below surface (dbs), and it was possible to advance a split spoon through the coarse material to a depth of 61.2 m dbs. A tricone was then advanced to get further into the till; however, at 62.1 m dbs it would not advance any further due to a cobble obstruction. A pencone was then advanced to determine depth to bedrock, whereupon bedrock was encountered at 64 m dbs. The pencone was advanced into bedrock to a total depth for the hole of 67.51 m dbs.

Visible and auditable gas in the form of percolating bubbles was released from the drill hole while extracting a Shelby tube from the hole. This gas was not tested in the field due to the quick and short lived release. Methane production in soils can occur when organic matter is degraded (Segers 1998), leading to a positive correlation between methane emission and organic matter. A large portion of methane emission globally comes from wetlands (Matthews and Fung 1987), indicative of the region the core was

63 L!1 !U

.».H

1 S-flJ .••• J iv "'ao-„^—ip

-U $#?i$i* !^#^.^&f

Plate 3.2: Lantech Drilling Services Inc. track mounted hollow stem augie r drill at drilling location (photo by P. Dickinson).

64 Plate 3.3: Split spoon with an inside diameter of 35 mm and length of 600 mm (photo by P. Dickinson).

65 "•"-' , '-V-Jfc

Plate 3.4: Shelby tubes with an inside diameter of 73 mm and length of 600-750 mm (photo by P. Dickinson).

66 extracted from. The gas release occurred between 17.0 m and 17.6 m dbs. Organics were recovered from 19 m and 16 m dbs, returning AMS dates of-7800 and ~7700 respectively. These dates correspond to the onset of the Hypsithermal warm period. The emitted gas was found in a silt; silt with sand; sandy silt section of the core. The gas was released upon retrieval of the core and stabilized after less than one minute of release.

Recovery information was logged for each core upon extraction and included information such as: sample depth, soil identification, sample number and remarks

(Appendix I). Drill information such as number of blows, penetration and length of recovered sample were also recorded. Hard plastic caps covered with plastic wrap and duct tape was placed on the end of each Shelby tube to prevent sample and moisture loss and reduce the possibility of contamination. Split spoon samples were extracted on site and then sealed in sections of PVC plastic tubing. Each core was labeled upon being sealed. The samples were brought indoors at the end of each day to keep them cool and avoid any abrupt changes in temperature. Samples were stored at the University of New

Brunswick, in the Department of Civil Engineering sediment lab at Head Hall, until the drilling and extraction was complete. A total of 94 sections of core were extracted, representing 67 Shelby tubes samples and 27 split spoon samples.

3.2 Laboratory Analysis - Procedures

Following completion of drilling, all Shelby tube samples were extracted at the

University of New Brunswick into split PVC pipe and measured (Plate 3.5). The core lengths were then split down the central axis using a guitar string (Plate 3.6),

67 >AJ

&*&r.>.^m

JKJ

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Plate 3.5: Core extracted into split PVC pipe (photo by P. Dickinson).

68 Plate 3.6: Core lengths split down the central axis using a guitar string. Diameter of core is 73 mm (photo by P. Dickinson).

69 photographed, and texture and sedimentary structures were described. Core samples were divided down the central axis as half the sample was used in laboratory analysis for this project, and the other half was retained for reference and further research. Following extraction laboratory analysis on the sediment began.

Analyses of the samples consisted of particle-size, atterberg limit determination,

X-ray diffraction, loss-on-ignition and ion chromatography analysis, as well as characterization of underlying sedimentary architecture with accelerator mass spectrometry radiocarbon dating of organics (Appendix II to VII).

3.2.1 Accelerator Mass Spectrometry Radiocarbon Dating

An accurate chronology must be developed before any interpretations can be made delineating the timing of landscape formation and palaeoenvironmental events within the Grand Lake Meadows and lower Saint John River valley. Changes to an ecosystem such as the breaching of a glacial lake or the introduction of marine waters into a river would have affected human land use. Therefore, the timing of such changes within the environment is important in understanding the human dimensions of adaptation to a changing landscape. Sediments are widely used to study environmental history, and one of the most important ingredients in such studies is an accurate chronology. The GLM-01 core was dated with one primary goal in mind; to establish the timing of past environmental change within the region.

During examination of the core 42 wood fragments and roots were encountered and collected for dating. Of these, 37 samples were large enough to obtain a radiocarbon date. Nine samples were submitted to IsoTrace Radiocarbon Laboratory, the University

70 of Toronto Accelerator Mass Spectrometry Laboratory, and one small sample (< 1 mg) to the Beta Analytic Radiocarbon Dating Laboratory, which did not return a date due to the small size of the sample. All samples submitted to IsoTrace have the same methods applied for preparation and chemical pre-treatment, which results in a typical precision of 0.2-0.3% being obtained for normal precision measurements that are a function of sample age (http://www.physics.utoronto.ca/~isotrace/).

All wood fragments initially found within the GLM-01 sediment core were extracted using clean metal tweezers, placed into a clean tinfoil bag, which was well labeled as to provienance. All samples were stored in a refrigerator that was set between

3-5° C. Prior to being sent to IsoTrace, samples were cleaned by extracting as much sediment as possible from the wood using clean metal tweezers. Samples were then placed on clean tin foil and weighed. Each sample was placed back into the original tin foil bag, which was then placed into a clean labeled plastic bag for shipping. Since some weight could potentially be lost due to laboratory pre-treatment of the wood the weight of the nine samples sent for dating were >10 mg. One sample weighed significantly <10 mg and did not return an AMS radiocarbon date.

When the dates were returned from the IsoTrace Laboratory (Appendix VII) the following description was included with their Accelerator Mass Spectrometry (AMS) radiocarbon dates:

These results are the average of 2 separate analyses (normal precision) and are corrected for natural and sputtering isotope fractionation, using the measured 13C/12C ratios. The sample ages are quoted as uncalibrated conventional radiocarbon dates in years before present (BP), using the Libby 14C mean life of 8 033 years. The errors represent 68.3% confidence limits.

71 Following international standards, unless otherwise specified, dates are presented as conventional dates in radiocarbon years BP (before present).

3.2.2 Laminae

Laminations are millimeter to centimeter thick strata distinguished in this project by differences in colour and particle size. Laminae consist primarily of allochthonous sediment and are typically thought of as the result of favourable seasonal sediment deposition, water stratification and lake circulation conditions (O'Sullivan 1983).

No microscopic or palynological examination was completed on specific laminae from this project and no laminae chronology was constructed using independent dating methods. However, a macroscopic laminae chronology was constructed for this project by counting only the clearly identifiable laminations. For this chronology each pair of one lighter, coarser lamination, and one darker, finer lamination was thought to equal one calendar year. Sediment from the light-coloured, coarser laminae was thought to have been deposited when the water was more turbulent permitting the suspension of coarser sediment and organics (spring, summer and fall months). The light-coloured laminae alternate with dark-coloured laminae, which are represented by finer sediment rich in organic matter. The finer sediment and organic material would more easily fall out of suspension during the winter months when there is less turbulence from the influx of water into the basin and/or ice cover (Smith 1978; Benn and Evans 2002). However, some of the laminae may not represent seasonal fluctuations but deposition from density driven undercurrents that carried terrestrially derived clastic sediment and organic matter

72 into the basin in response to brief storm events that mobilized loose sediment from the headwaters and sides of the drainage basin as debris flows.

Since the actual cause of the laminae is unknown and the chronology is not supported by AMS radiocarbon dating the laminae chronology is not used in the final analysis or interpretations. Additionally, the laminae chronology is based on the assertion there were a number of possible errors in counting and the determined number of years would be a minimal number.

3.2.3 Particle Size Analysis (Hydrometer)

Particle (grain) size analysis was carried out on the <2 mm size fraction using analytical sieves for the coarse end of the particle-size spectrum (sand size or larger) and hydrometers to test the silt and clay. The particle size distribution of the soils was completed according to procedures and methods described in the American Society for

Testing and Materials Method D 422-63 (ASTM 1992) in the Soils Laboratory,

Department of Civil Engineering, University of New Brunswick. Analytical sieves were carried out on 153 samples ranging from 0.3 to 60.4 m dbs. This method determined the percent gravel and sand, and grouped the silt and clay together as fines. Hydrometer tests were completed to differentiate the percent silt and clay on 104 samples ranging in depth from 18.5 to 59.2 m dbs. On average particle size and hydrometer testing was determined on a sample every 40 cm throughout the core.

73 3.2.4 Atterberg Limit Determination

Atterberg limits were completed for 77 samples from a depth of 18.5 m to 59.2 m dbs, an average of one sample every 53 cm. These geotechnical tests indicate the upper and lower limits of the range of water content over which a soil exhibits plastic behaviour

(Craig 1997). The liquid and plastic limits were derived from test procedures and methodology described and referenced in ASTM D 4318-00 (Method A) (2000). All tests were completed in the Soils Laboratory, Department of Civil Engineering,

University of New Brunswick. The material was allowed to air dry prior to testing.

Determinations of the plasticity index, liquidity index and activity with depth were conducted.

The liquid limit is defined as the water content of a soil, expressed in percent, dry weight, having a consistency such that two sections of a soil cake, placed in a cup and separated by a groove, barely touch but do not flow together under the impact of several sharp blows (Gillott 1968, p. 10). Liquid limit is the percent water content of a soil at the arbitrarily defined boundary between the liquid and plastic states. The plastic limit is defined as the water content, expressed in percent, dry weight, at which a soil will crumble when rolled into a tread 3 mm in diameter (Gillott 1968, p. 10). The plastic limit is the percent water content of a soil at the boundary between the plastic and brittle states.

The plasticity index is the range in moisture content over which the soil behaves plastically and is defined by the difference between the liquid limit and the plastic limit

(Gillott 1968, p. 10). The liquidity index is obtained by calculation from the natural moisture content, the plastic limit and the liquid limit. The determination of liquid and plastic limits included the measuring of natural water content. Atterberg limit

74 determinations for the 77 samples from the GLM-01 core were not used in the final analysis or conclusions as they were conducted only to aid in comparison with other research completed in the lower Saint John River valley (Daigle 2005; Guidice 2005).

3.2.5 X-Ray Diffraction Method

X-ray diffraction (XRD) was used as it is a nondestructive qualitative analysis allowing the sediment to be later used for other analyses if desirable. Samples were analyzed in the X-Ray Diffraction Laboratory, Department of Geology, University of

New Brunswick, using standard operating procedures by a Bruker D8 Advance Solid

State Power Diffraction XRD system (S. Boonsue, personal communication 2008).

Each sample supplied for analysis was ground to a fine particle size using a non- percussive technique. A non-automated method of grinding was completed that included grinding by hand with a mortar and pestle. For rapid determination of accurate peak positions (phase identification), Plexiglas top-load mounts were used. For phase identification, top loading of a thick powder sample of randomly oriented crystallites was employed, which helped to minimize preferred orientation. The powder was loaded into the well and leveled with a flat-edged tool. This produced a well packed specimen which presented a very flat surface to the beam. The samples were prepared as bulk samples.

All the samples were run for the same time with the same step size in 2 theta, with the same accelerating voltage and sample current.

Results were returned for 52 sediment samples located between 19.2 and 58.8 m dbs. Samples were taken for analysis on average every 79 cm determining if the minerals quartz, muscovite, albite, clinochlore, calcite, orthoclase and vivianite were present. X-

75 ray diffraction for the 52 samples from the GLM-01 core were not used in the final analysis or conclusions as they were conducted only to aid in comparison with other research completed in the lower Saint John River valley (Daigle 2005; Guidice 2005).

3.2.6 Ion Chromatography

Two soluble anions that are commonly determined in saline soils are chloride (CI) and bromide (Br). The CI and Br content were determined for 147 clay and clayey silt samples. These samples were extracted on average every 40 cm throughout the core ranging in depth from 0.3 to 59 m dbs. The CI and Br concentrations were determined on a Dionex, DX-120 ion chromatograph (IC), located in the Hydrology Laboratory,

Department of Geology, University of New Brunswick using method 4110 (Eaton et al.

1995). The concentrations of CI and Br in the soil water were corrected using the gravimetric water content (Stone 1984; Murphy et al. 1996), according to the equation:

Clsw = fCl in extract (ug/gH?0)l [Milli-0 water fgFbOII

[dry weight of soil (g)] / [Moisture content (gl-^O/g dry soil)]

For each test sample approximately 5 g of dried sediment sample was mixed with

10 g of Nanopure water in a clean plastic bottle. A 1:2 ratio of sediment to water was used as a 1:1 ratio did not allow for the extracted water to pass through the filter paper.

Each sample was shaken for 24 hours and then allowed to set for 1 hour prior to extraction of the fluid with a pipette and syringe. The fluid was then extracted through a

0.45 urn syringe filter prior to the chemical analysis. Standard anion concentrations were used to calibrate the system. A number of triplicates, blanks and duplicates were run throughout testing to be sure the methodology was sound. Triplicates were run

76 approximately every 25 samples, a method blank was run every 3 days and a duplicate was run every 15/20 samples, with the fluid extracted split just prior to the IC run.

3.2.7 Loss-on-Ignition

Loss-on-ignition (LOI) is the main laboratory technique used to measure the organic matter content of soils and sediments. Although many different methods are available, they are all based on the principle that the weight lost on heating at a defined temperature is closely correlated with the organic matter content of the sample.

There are a number of recommended methodologies for loss-on-ignition, all very similar with only slight changes in the time of burn (Dean 1974; Heiri et al. 2001; Smith

2003). The accepted LOI procedure consists of samples being weighed to calculate original weight (W), then dried (Wd) atT05°C to remove moisture (Mc = W - Wdjos), and finally burned at 550°C to calculate LOI (LOI = Wdi05 - Wd55o). It has been demonstrated that the Wdsso weight represents ignition of all organic compounds in the sample. The methodology used in this analysis for LOI followed Dean (1974).

However, after a number of test runs there was a modification to Dean's (1974) methodology of burning the samples at 550°C for one hour, with samples from the GLM-

01 core burned at 550°C for two hours. A total of 489 samples were run for LOI in the

Magma and Mineral Synthesis Laboratory, Department of Geology, University of New

Brunswick. The samples ranged in depth from 0.3 to 62 m dbs, with a sample taken every 12.8 cm throughout the length of the core.

Samples were run in a series of 16 samples per burn. Crucibles were weighed to determine the mass of the container and sediment samples were then added to the

77 containers. Individual samples were stored in air tight containers until LOI analysis began. The wet samples were placed in crucibles and then weighed. Once the mass was recorded, the samples were placed in a drying oven over night (-16 hours) at a temperature ranging between 100 to 105°C. The samples were then removed from the oven and allowed to cool to room temperature (-30 minutes) in a desiccator. When the samples reached room temperature, they were pulverized in their crucibles and were again weighed. The average weight of the dried sample was 2 g. Once the mass of the oven dried samples was recorded the samples were placed in a 550°C high temperature, controlled atmosphere Naberthem Mosiz resistance furnace and burned for two hours.

The temperature was controlled by a type B thermostat accurate to 2°C according to

NIST standard (±2° C). The samples were then removed from the oven and allowed to cool to room temperature (-30 minutes) in a desiccator. When the samples had reached room temperature they were again weighed to determine the amount of mass lost as the organics in the sample were burned off. LOI was then calculated using the following equation:

LOI550 = ((DW,o5 - DW550) / DW105) x 100

Where LOI550 represents LOI at 550°C (%), DW105 represents the dry weight of the sample before combustion and DW550 the dry weight of the sample after heating to 550°C

(weight in g).

A concern with the LOI technique is that some clay minerals will lose structural water at the temperatures used to combust the samples. The structural water loss will increase the total sample weight loss leading to an overestimation in organic matter content. One possible means to avoid this concern is through the pre-treatment of the

78 sample via removal of the mineral matter using HCI acid; however, the use of HCI may dissolve part of the organic matter leading to an underestimation of the organic matter content (Schumacher 2002).

Therefore, without pre-treatment it is likely that the LOI analysis will slightly overestimate weight loss due to the liberation of small quantities of structural water from clay minerals. It has been determined by Smith (2003) that significant additional weight loss occurs in the burn process between 2 and 2.5 hours in clay-rich samples. Smith

(2003) suggests that the reason for this sudden increase in LOI after 2 hours appears to be the build-up of a surface crust during heating that insulates the core of the sample from ignition temperatures. After 2 hours this crust breaks down and exposes the sample core to ignition temperatures increasing weight loss. Therefore, if the burn process is <2 hours the overestimation of LOI due to loss of structural water is thought to be insignificant with a difference of <0.25% (Smith 2003).

3.2.8 Natural Moisture Content

The natural moisture (water) content was determined for all sediment samples upon extraction of the cores, prior to all other analysis. Natural moisture content was derived from test procedures described and referenced in ASTM D 2216-98 (1998). All tests were completed in the Soils Laboratory, Department of Civil Engineering,

University of New Brunswick. The mass of the clean dry specimen containers was determined using a measuring scale and recorded. Wet samples were extracted into the specimen containers and a record of the depth the sediment sample was extracted from was recorded. The mass of the moist test specimen with container was determined and

79 recorded. The container with the moist material was then placed in the drying oven and dried overnight to reach a constant mass (~16 hours). The drying oven temperature was set at 110° C. The mass of the dry sample with container was then recorded. The mass of the wet sample with container was then subtracted from the mass of the dry sample with container to determine the weight of the water (A). The weight of the dry sample

(B) was determined by subtracting the weight of the dry sample with container from the weight of the empty container. The natural moisture content (given as a percentage) of each sample was then calculated using the following equation: (A / B x 100) where A represents the weight of water and B represents weight of dry sample (weight in g).

3.3 Results of Laboratory Analysis

Laboratory work for the GLM-01 sediment core consisted of geotechnical analysis that included moisture content tests, particle size analysis and atterberg limit determination. Additional analysis included ion chromatography, loss-on-ignition and x- ray diffraction. Accelerator Mass Spectrometry was completed on organic wood fragments found throughout the sediment core. Also, a conservative estimate of number of laminae was determined to help obtain additional environmental information that may be contained within the sedimentary record.

3.3.1 Accelerator Mass Spectrometry Radiocarbon Dates

A total of nine AMS radiocarbon dates were obtained from organic wood fragments to provide the chronological framework for the top 28.68 m of the GLM-01 core (Table 3.1). Eight of the nine dates were found to increase in age sequentially from

80 110.36 ±0.70 years BP (TO-13063) (all dates given are uncalibrated) at 0.71 m to

11,340 ±210 years BP (TO-13071) at a depth of 28.68 m. All the material dated was wood material. A sample of wood collected at a depth of 41.97 m was too small from which to obtain an AMS date.

Sample Radiocarbon Laboratory Calibrated age Sample depth (m) date (yr BP) number (yr BP) description 0.71 110.36±0.70 TO-13063 1960 AD (1999 AD) wood 6.02 3080±70 TO-13064 (1325)1385 wood 10.21 3820±60 TO-13065 2210(2215)2230 wood (2245)2280 12.62 4770±70 TO-13066 3530 (3560)3565 wood (3570) 3575 (3630 16.59 7770±80 TO-13067 6600 wood 19.81 7820±90 TO-13068 6645 wood 22.68 9600±110 TO-13069 8920 (8995) 9120 wood 25.6 8150±80 TO-13070 7080(7110)7120 wood 28.68 11,340±210 TO-13071 11,270 wood Table 3.1: Details of AMS radiocarbon-dated samples from the GLM-01 core.

There are a number of books and articles that go into great detail discussing the various factors which affect the accuracy of radiocarbon dates (Barker 1972; Coleman and Fry

1991). Despite some of these limitations the method is still a very important scientific aid to research.

3.3.2 Laminae

Laminations, millimeter to centimeter thick strata, were distinguished on wet sediment in the GLM-01 core by differences in colour and particle size (Plate 3.7). Such structures were common throughout the sediment core between 35.1 to 59.3 m dbs.

Laminations were identified sporadically throughout the core between 15.2 to 35.1 m dbs. Normalized, the number of laminae per 610 mm was 2850 (Figure 3.3).

81 Plate 3.7: .Laminations on wet sediment in the GLM-01 core. Diameter of core is 73 mm (photo by P. Dickinson).

82 Varves per 610 mm 0 20 40 60 80 100 120 140 160 180 200

_l I I I I I L.

£ 30 .-•-•-•-•-•

'•••*•- 60

Figure 3.3: Summary of results of laboratory testing with dots depicting laminae normalized per 610 mm compared with depth.

83 3.3.3 Particle Size Analysis (Hydrometer)

For the top 18.5 m and bottom 1.2 m of the GLM-01 core 48 sediment samples were analysed for particle size as discussed in the methods above. Hydrometer tests were completed on 104 sediment samples from 18.5 to 59.2 m dbs to determine the percent each of sand, silt and clay (Figure 3.4).

The top 4.9 m of the core was predominantly silt and clay with a high of 98.1% at

1.6 m dbs. The particle size increases dramatically at 4.9 m to 99.8% sand. From 4.9 to

15 m dbs the particle size is mostly sand with fluctuations from 99.8 to 51.7%. At 15 m dbs the percent silt and clay increases dramatically again to 97.7%.

As the percent of silt and clay continues to be high for most of the remainder of the sediment core at 18.5 m dbs hydrometer tests begin and continue to 59.2 m dbs. The percent sand fluctuated from a high of 23.5% to no sand being present, decreasing as depth below surface increases. Silt follows this same trend with a gradual decrease as depth increases. The percent silt ranged from a high of 92.1% at 24.5 m dbs to a low of

41.4% at 52.7 m dbs. As sand and silt decrease the percent clay increases from a low of

2.3% at 24.5 m dbs to a high of 78.3% at 53.5 m dbs. At 53.5 m dbs clay starts to decrease to a low of 24.9% at 58.1 m dbs. The range of sand for the last meter of the sediment core was between 8 and 53.3% with a clay and silt range between 14 and

46.7%. From the description of the particle size analysis the stratigraphy for the GLM-01 sediment core was determined.

84 Figure 3.4: Summary of results of hydrometer tests depicting the percent each of sand, silt and clay with depth.

85 3.3.4 Atterberg Limit Determination

The liquid limit for the samples tested from the GLM-01 core ranged from 19 to

41, with an average liquid limit of 28.6 (Figure 3.5). The plasticity index from the GLM-

01 core ranged from non-plastic to a plasticity index of 13. Nineteen samples tested were non-plastic. The non-plastic sediment was found primarily between 18.5 and 26.4 m dbs, and at 29.4 and 58.6 m dbs respectively.

3.3.5 X-Ray Diffraction

X-ray diffraction was the analytical technique used to determine the mineralogy of the fine-grained sediments from the GLM-01 sediment core to help determine if the region underwent marine, brackish or freshwater submergence. Results of the analysis indicated sediment with a mineralogical composition consisting of quartz, muscovite, albite, clinochlore, calcite and orthoclase (Figure 3.6). Through macroscopic observation of the sediment along the core after extraction and splitting, small bright blue sediment concretions were observed. The concretions were often up to 5 mm in size (Plate 3.8).

Additionally, these concretions were observed surrounding or in association with some of the organic fragments that were obtained for AMS dating (Plate 3.9). X-ray power diffraction was used to confirm that a sample of the blue sediment concretions (extracted from a depth of 41.5 m dbs) corresponded to the mineral vivianite (Fe3+3(P04)28(H20)).

The vivianite was noted along the sediment core between 15.9 to 42 m dbs (Figure 3.7).

86 Atterberg Limits (%) 15 25 35 45 " 55

Figure 3.5: Summary of results of laboratory testing depicting variation of liquid limit, plastic limit and natural water content with depth.

87 Mineralogy Quartz Muscovite Albite Clinochlore Calcite Orthoclase 0 -i

10-

• I • 1 • • • • t 1 C O K > O i 1 1 1 t I ! 1 •

Dept h (m ) • • • 40 - i • • • • • 1 ! s ! 1 i • • • • • 50- • I I j 1 ! 1 t • t i i i I 60 - 1 •

Figure 3.6: Summary of results X-ray diffraction testing depicting variation in mineralogy with depth.

88 Plate 3.8: Photograph of the mineral vivianite (blue) at 19 m depth below surface. Diameter of core is 73 mm (photo by P. Dickinson).

89 Plate 3.9: Photograph of the mineral vivianite (blue) found in association with organics at 40 power, 2.5 m depth below surface (photo by P. Dickinson).

90 Occurance of Visible Vivinite

0 -I

20 - I

-§- 30 - I +•» Q. ! Q 40 - I

50 -

60 -

Figure 3.7: Summary of results depicting vivinite location with depth.

91 3.3.6 Ion Chromatography

While chloride concentrations were measurable throughout the GLM-01 sediment core (Figure 3.8), bromide concentrations were undetectable in three locations, between

3.2 and 8.6 m dbs, at 56.7 m dbs and between 58.2 and 59 m dbs (Figure 3.9). The chloride concentrations ranged from a low of 2.4 mg/L at 96.5 cm dbs to a high of 303.2 mg/L at 38.2 m dbs. The CI/Br ratio could not be determined in the locations where bromide concentrations were below the detection limit or <0.5 mg/L. The highest CI/Br ratios were found in the lower half of the core; however, they did fluctuate throughout the remainder of the core (Figure 3.10). Where they could be determined the CI/Br ratios were as low as 2.78 at 96.5 cm dbs and reached a high of 219.50 at 48.1 m dbs.

3.3.7 Loss-on-Ignition

LOI data shows that the percent organics in the core from bedrock to surface range from 0.8 to 6% (Figure 3.11). The lower portion of the core (-54 to 62 m dbs) is characterized by a decreasing percentage of organics ranging from 0.8 to 4.75%, with just a slight increase at 62 m dbs from 0.8 to 1.11%. This slight increase is found at the bottom of the core just above bedrock. There is a slight increase in organics between 52 to 54 m dbs from 3 to 4.7%. The middle portion of the core (-15 to 54 m dbs) contains a relatively stable percentage oTorganics (~3%) with a range between 2.2 to 4.3%. At

-15 m dbs there is a large increase in the percent of organics from 1 to 4.3%. This is followed by 7.5 m of relatively stable percentages with a minimum value of-1% and a high of-1.7%, which occurs at a depth of-14 m dbs. The upper -7 m of the core is characterized by a decrease in organics from 6% at the surface to 1% at 7.5 m dbs.

92 Chloride Corrected (mg/l) 50 100 150 200 250 300 350 V iiii 10

• — * «-**

£ 30 T~;—* *—•«-• 4-a*

Figure 3.8: Summary of results of the ion chromatography tests depicting the chloride content (mg/L) with depth.

93 Figure 3.9: Summary of results of the ion chromatography tests depicting the bromide content (mg/L) with depth.

94 CI/Br Ratio 50 100 150 200 250

V •

S- 30 I 40

Figure 3.10: Summary of results of the ion chromatography tests depicting the chloride and bromide ratio with depth.

95 Figure 3.11: Summary of results of the loss-on-ignition tests depicting the amount of organic material with depth.

96 LOI fluctuated throughout the sediment core; however, there were four regions where LOI went from either relatively low to relatively high with little change in depth.

From 54.8 to 53.8 m dbs LOI increased from 3.2 to 4.75%. At 15.3 to 15.1 m dbs LOI decreased from 4.3 to 1.26%. There was a large increase of LOI at 1.85 m dbs with a percentage of 8.41 %. This increase in organics was due to the sample being taken from inside what has been interpreted as a ~1 cm thick rodent burrow filled with organic material. Finally, there is an increase in LOI from 0.9 to 0.3 m dbs with LOI between

2.26 and 6.12%.

3.3.8 Natural Moisture Content

The natural moisture content was determined to be lowest just above the bedrock (Figure 3.12). Moisture content increases quickly as depth below surface decreases from a low of 21% at 59 m dbs to a high of 40% at 52 m dbs. Throughout the remainder of the sediment core the moisture content averages 33%. However, at 8 m dbs the moisture content decreases to 22%, similar to that found just above bedrock. At both locations coarse-grained sediment, that contained little fine material, was identified.

3.4 Interpretation of Laboratory Analysis

An interpretation of the results generated for each of the laboratory analysis introduced in section 3.3 is presented.

97 Moisture Content (%) 15 20 25 30 35 40 45 50

fl i i .1 i i i \J •'•„*• .- • • • •• • 10 -

• •*• • # 20 -

.;*•*•••• •**•• ^^ : ••• \v •• • i. 30 - • •• • • Dept h 40 - «••

50 - • • i* • • • • • ••**• 60 -

Figure 3.12: Summary of results of the natural moisture tests with depth.

98 3.4.1 Accelerator Mass Spectrometry Radiocarbon Dates

The dated material allows for chronological control to be obtained associated with basin and landscape change, as well as the timing related to the spatial distribution of archaeological remains and possible past human activities for the region. The oldest date is considered to represent a minimum finite-age of the basin. As the oldest finite date was recovered from the upper half of the total depth of water-lain sediment, the basin is likely much older in age.

One of the nine dates did not fit the otherwise linear pattern of radiocarbon dates obtained. Figure 3.13 represents each of the measured dates, including their confidence interval to 1 standard deviation. The results of a linear regression are also shown by a dotted line. The 8150 ±80 years BP (TO-13070) date obtained on wood found at 25.6 m dbs was slightly younger than the 9600 ±110 years BP (TO-13 069) date obtained at

22.68 m dbs. However, using 2 standard deviations with a 95% probability indicates that the true (radiocarbon) age of the 8150 ±80 years BP (TO-13070) date is between 7990

BP and 8310 BP, placing it between the 7820 ±90 years BP (TO-13068) and 9600 ±110 years BP (TO-13 069) dates, fitting it strati graphically within the chronology obtained by the other eight radiocarbon dates.

It is possible that turbation mixed the organics stratigraphically. Distinct visual laminations within the sediment were not present between 22.11 and 28.04 m dbs.

Therefore, the 8150 ±80 years BP (TO-13070) and the 9600 ±110 years BP (TO-13069) dated material were both within an area where there is no visible undisturbed banding of the sediment suggesting a potential dating error associated with turbation, possibly due to subaqueous slumping or bioturbation.

99 Radiocarbon Date (Years BP) 0 2000 4000 6000 8000 10000 12000 14000 U " •^ ""». Best Fit Line using Linear Regression *>• • R squared = 0.94 10 -

'— 4» 20 -

m -i- 30 - .c Q. W Q 40 -

50 -

60 -

Figure 3.13: Summary of results of each of the measured dates (including the confidence interval to 1 standard deviation) with depth.

100 3.4.2 Laminae

Although laminations are frequently identified in lacustrine sediments, rhythmically laminated deposits can also be found in marine sediments (Powell 1981;

Gilbert 1982; Domack 1984; Mackiewicz et al. 1984; Miall 1985; McCabe 1986; Cowan et al. 1988). Often in non-marine sediments coarser particles fall out of suspension during the melt season to form the lower layer of clastic laminae (varve), while the finest particles are held in suspension until calm water conditions prevail, usually under ice cover. Laminae cannot be considered varves unless it is clearly demonstrated that there is annual deposition. With regards to the GLM-01 core it cannot be clearly demonstrated that the laminae are related to annual deposition, therefore they could not be used to help develop the chronology of the Grand Lake Meadows.

There are a number of possible sources of error in laminae interpretation.

Determining what is laminae in a given sedimentary record may introduce subjectivity. It is possible to have laminae counting errors, either with missed laminae or the addition of extra laminae. This could be the result of localized sedimentation variability, sediment disturbance, vague sediment structures or human error.

A number of fluid structures were noted throughout the center of the GLM-01 sediment core (i.e. Plate 3.10) particularly between 34 and 58 m dbs. Such structures were likely the result of compression of the sediment during the initial drilling process and/or from compression during the extraction of the sediment core from the Shelby tubes. It is highly likely that missed laminae were common in these disturbed segments of the core, due to the laminae typically being less discernible than in other undisturbed sections. Therefore, due to the subjectivity of determining the number of laminae and the

101 1

Vr^^t...^..^.

Plate 3.10: An example of a fluid structure found throughout the core. Diameter of core is 73 mm (photo by P. Dickinson).

102 possibility of counting errors in the sedimentary record, the laminae record is not considered to represent an accurate record of deposition.

3.4.3 Particle Size Analysis (Hydrometer)

The differences in percent sand, silt and clay in the lower portion of the core demonstrate major changes in depth of water over the region. Fines (silt and clay) continue to increase from just above the till to a high at -53 m dbs when there is deep water sedimentation over the lower river valley. There are fluctuations in grain size between sand, silt and clay in the lower half of the core, with gravels introduced from

~16 to 7 m dbs, indicative of faster flowing water through the region. At ~6 m dbs gravel is no longer present in the GLM-01 sediment core and fines (silt and clay) again increase.

These fines, below and above the gravel, are indicative of slower moving water over the region.

3.4.4 Atterberg Limit Determination

Gillott (1968, p. 11) suggests that there is a relationship between the liquid limit and plasticity index for glacial clays, with the liquid limit range between 21 and 72 and the plasticity index range between 8 and 45. The liquid limit from the GLM-01 core ranged from 19 to 41 with the liquid limit just below Gillott's (1968, p. 11) glacial clay range in two locations tested. The liquid limit at 57.8 m dbs was 19 and at 58.6 m dbs it was 20. The liquid limit from the Fredericton Junction and Fredericton core locations were within Gillott's (1968, p. 11)21 to 72 liquid limit range for glacial clays. The

103 average liquid limit for the samples tested from the GLM-01 core was 28.6, at the lower half of Gillott's (1968, p. 11) range for glacial clays.

The plasticity index from the GLM-01 core ranged from the sediment being non- plastic to having a plasticity index of 13, again at the lower end of Gillott's (J 968, p. 11) range for glacial clays. Nineteen samples tested were non-plastic, indicative of silt with no clay content. The non-plastic sediment was found primarily between 18.5 m and

26.4 m dbs, the upper portion of the sediment core. Two other locations tested also indicated non-plastic sediments, at 29.4 and 58.6 m dbs. The only samples from the core that were within Gillott's (1968, p. 11) 8 to 45 plasticity index range were the four samples taken between 52.4 to 54.3 m dbs. Therefore, the only section of core that falls within Gillott's (1968, p. 11) liquid limit and plasticity index range for typical glacial clay is the area between 52.4 to 54.3 m dbs. Both the liquid and plastic limits of the sediment tested generally show a rise when depth increases, with a slight decrease just above the bedrock.

In general the natural moisture content is higher where the stratigraphic unit has been identified as clay and lowest where coarse material has been identified. Therefore, variations in natural moisture content with depth may well be attributed to a change in grain size with depth.

3.4.5 X-Ray Diffraction

The clay minerals identified through the XRD analysis of the GLM-01 core were muscovite and clinochlore. Muscovite, part of the phyliosilicate (clay) subclass (Klein and Hurlbut 1993), is found in many silicic to intermediate igneous rocks such as granites

104 and pegmatites, as well as in a wide variety of metamorphic rocks, and some sedimentary rocks such as sandstones (Deer et al. 1996; Perkins 2001).

Olinochlore is a member of the chlorite clay group of minerals and is common in argillaceous sedimentary rocks, which can be found in the Carboniferous shale and sandstone units that underlie much of the lower Saint John River valley (Weaver and

Polland 1973; Velde 1985; Deer et al. 1996; Perkins 2001). The origin of the clay minerals muscovite and clinochlore in the samples tested from the GLM-01 core could be due to glacial erosion of the underlying bedrock. However, Monro (1994) reported the presence of clinochlore in a lacustrine clay sample collected from the Fredericton

Regional Landfill.

Most of the minerals identified through XRD are silicate minerals, which are often common and abundant minerals occurring in a great variety of geological environments. Therefore, most are not useful as a tool for the identification of a specific depositional environment. Allen and Johns (1960) suggest that source material has a greater effect on the mineral composition of the sediments than the environment in which it was deposited.

Quartz, orthoclase and albite are widely distributed in igneous, metamorphic and sedimentary rocks and dominate in sandstone (Perkins 2001); therefore, they are difficult to use as an indicator of a specific depositional environment. The occurrence of calcite could also be due to the surrounding rocks of the Carboniferous Basin. Calcite is a common cementing medium in clastic sedimentary rocks (Klein and Hurlbut 1993; Deer etal. 1996).

105 Allen and Johns (1960) conducted petrographic studies and XRD analysis on

Quaternary clay samples from Fredericton and Saint John and found that calcite was not detected in any of the samples. However, it was noted that calcite does occur in shale and clay of both marine and non-marine origin; therefore, they determined that calcite was deposited through secondary deposition by carbonate solutions (Allen and Johns

1960). Calcite was not a reliable indicator of a clay depositional environment.

XRD analysis was completed by Giudice (2005) on clay-silt samples from sediment cores from Fredericton and Fredericton Junction. The mineral composition was similar between both cores except calcite was absent from the Fredericton Junction data set. The mineral composition from the GLM-01 core, in the present study, is most similar to core analysis from the Fredericton area (Daigle 2005). Since calcite was not present in the Fredericton Junction data set, and the sediment source for all three cores is thought to be the same, the origin of the calcite in the Fredericton and GLM-01 core may be due to something other than the Carboniferous calcite-bearing bedrock. Since calcite may be representative of a marine or brackish water depositional environment, Giudice

(2005) suggests that the deposition of freshwater glaciolacustrine sediment was the major process in the Fredericton Junction area. Therefore, it is likely that the source of calcite found in the Fredericton and GLM-01 core was supplied by the post-glacial marine inundation in the region. Perkins-(2001, p. 33) suggests that inland lakes or seas commonly precipitate calcite.

Quartz, orthoclase, albite, muscovite, calcite and clinochlore could all be eroded from the bedrock found in the Saint John River valley, from the Chaleur Uplands to the

New Brunswick Lowlands. Therefore, from mineral analysis of the GLM-01 sediment

106 core it is difficult to say conclusively that, other than vivianite, the minerals identified through XRD analysis are attributable to anything other than the deposition of glacial sediments scoured from local bedrock.

The vivianite concretions from the GLM-01 core occur in the silt- and clay-rich sediments and are common in the well-laminated sections of the core. This would suggest that vivianite formation in these areas was related to the input of suspended sediments.

In lakes, the formation of vivianite could be either authigenic or diagenetic. In the first case vivianite is generated where it is observed and is a characteristic of sedimentary minerals found during sedimentation. However, if the vivianite were to be diagenetic then it is related to a chemical, physical or biological change undergone by sediment after its initial deposition and during and after its lithification. Evidence suggests that the vivianite concretions are related to authigenic not diagenetic processes as they are associated with areas of high biological productivity where the organics were able to fall out of suspension with the fine silt and clay. Additionally, the vivianite was not associated with an oxidized layer or crust, but found only as small concretions. Deike et al. (1997) noted that vivianite production is most likely to be formed just below a thick oxidized layer if related to a diagenetic formation.

3.4.6 Ion Chromatography

Freshwater, brackish water, saline water and brine all contain specific amounts of dissolved salts (Table 3.2). Freshwater contains low concentrations of dissolved salts with brackish water saltier than freshwater, but not as salty as seawater. Brackish water

107 may result from mixing of seawater with freshwater, as in estuaries, or it may occur in brackish fossil aquifers (Giudice and Broster 2006). Saline water is water that contains a significant concentration of dissolved salts, and brine is water saturated with, or containing, large amounts of salt.

Total dissolved solids mg/L Degree of salinity 0-1000 Fresh: non-saline 1001-3000 Slightly saline - > brackish 3001 - 10,000 Moderately saline - > brackish 10,001-100,000 Saline > 100,001 Brine Table 3.2: Dissolved solids-salinity relationships (McNeely et al. 1979).

Seawater has a salinity of-3.5%, or 35 parts per thousand. Saline water has a relatively high concentration of dissolved salts (cations and anions) with 11 main salt ions making up 99.9% of seawater (Table 3.3). Two of the ions in seawater examined as part of this study are chloride and bromide.

Chemical ion Concentration, ppm, mg/kg Part of salinity % Chloride CI 19,345 55.03 Sodium Na 10,752 30.59 Sulfate S04 2701 7.68 Magnesium Mg 1295 3.68 Calcium Ca 416 1.18 Potassium K 390 l.ll Bicarbonate HC03 145 0.41 Bromide Br 66 0.19 Borate B03 27 0.08 Strontium Sr 13 0.04 Fluoride F 1 0.003 Table 3.3: The 11 main salt ions of seawater (from Hem 1989, p. 7).

The absorption of chloride and bromide onto the surface of the clay minerals was used as a possible indication of brackish or marine water deposition. In saline soils chloride anions are found in a greater abundance than bromide anions (Burt 2004).

While chloride concentrations were measurable throughout the GLM-01 sediment core,

108 bromide concentrations were found to be undetectable in areas close to the bottom and close to the top of the sediment core. Seawater contains 19,000 to 20,000 mg/L of chloride (Morris and Riley 1966; Manheim 1972). Davis et al. (1998, 2000, 2001) have indicated that the chemical ion ratios of chloride/bromide are especially useful as geochemical indicators in assessing marine inputs to a region, with seawater having a

CI/Br ratio of 290 (Morris and Riley 1966; Manheim 1972).

There are a number of ways water can become saline, such as:

1. groundwater circulating in rock formations can acquire the chemical signature

associated with the rocks;

2. modern sources such as industrial and agricultural runoff and salt used for deicing

roads in the winter;

3. pockets of relict seawater;

4. chloride is an important component of precipitation due to the influence of sea-

spray on local atmospheric conditions; and

5. seawater intrusion from late glacial marine inundation of the region.

One way water can become saline is by coming into contact with soil or geologic material that is high in salts. This occurs through the dissolution of evaporitic deposits such as halite (rock salt), anhydrite, and gypsum (Manheim and Horn 1968; Meisler

1989). Frape et al. (2004) identified CI/Br ratios in a range of fluids from crystalline rocks across several continents and found these values to range quite widely form ~25 to

1000. However, Frape and Fritz (1987) found the CI/Br ratios for subsurface rocks are more typically -200. Whittemore (1995) and Davis et al. (1998) found that the CI/Br ratio was over 10,000 for solutions from the dissolution of marine evaporates. The CI/Br

109 ratio in halite is 1 to 2 orders of magnitude higher than in seawater (Braitsch 1971), with the CI/Br ratio for seawater approximately 290 (Morris and Riley 1966; Manheim 1972).

The range of the CI/Br ratio for the sediment in the GLM-01 core is from 150 to 300.

The GLM-01 sediment core is well within the area of Carboniferous bedrock, which in New Brunswick is represented by both Mississippian and Pennsylvanian strata.

Since the Pennsylvanian strata are represented by fluvial-lacustrine-deltaic environments

(Hamilton 1961) the occurrence of coal deposits precludes the existence of widespread aridity, which would be necessary for extensive evaporate formation (Webb 1981).

Commonly CI/Br ratios in excess of 2000 reflect the dissolution of halite (Davis et al.

2001) and any brines resulting from evaporate dissolution have a CI/Br ratio ranging from 1500 to 15,000 (Cecil 2000). Also, since the Mississippian elastics that do contain potash-bearing evaporate material are generally overlain or capped by volcanics, this would protect them from later erosion (Hamilton 1961).

Water can also become saline due to pollution from various anthropogenic

(human based or human sourced) sources including sewage and some industrial effluents, oil and gas-field brines brought to the land surface during exploration and production, road deicing salts, and return flows of irrigation water. Many anthropogenic sources of chloride, such as sewage, have high CI/Br ratios (Vengosh and Pankratov 1998).

Additionally, water with a very high CI/Br ratio but a moderate CI content is indicative of road salt or agricultural chemical pollution (Davis et al. 2001). The areas throughout the

GLM-01 sediment core that had the highest CI/Br ratios also had the highest CI content.

However, such an anthropogenic contribution cannot be entirely ruled out based solely on chloride concentrations. In such cases, however, CI/Br ratios can be very useful in

110 assessing modern chloride sources. Anthropogenic chloride from industrial processes, agriculture/fertilizer run off and road salt is tagged with notably higher CI/Br ratios

(above 300) (Davis et al. 2001), close to seawater (Cl/Br=290). The highest CI/Br ratio identified in the GLM-01 core is 219.5, at a depth of 48 m dbs, consistent with pre- anthropogenic CI/Br ratios. Additionally, Snow et al. (1990) determined that bromide is not typically part of the chemical composition for road salt. Therefore, the CI/Br ratios for the GLM-01 core have not been significantly impacted by human activity.

Reviews of borehole logs, geophysical logs, and water analysis data, located throughout southern and central New Brunswick, by Giudice and Broster (2006), Webb

(1981) and Roy and Elliott (1980), indicates that some deeper aquifers are commonly found to have high chloride concentrations. Giudice and Broster (2006) give an explanation for the origin for the saline water interpreting the pockets of brackish water found within the lower Saint John River valley as remnants of trapped sea water from the

DeGeer Sea inundation following the retreat of the Late-Wisconsinan ice sheet from the region. They further suggest that it could be expected that pockets of relict saline groundwater could be found in valleys that were glacially over-deepened and inundated by marine waters. Webb (1981) also suggests that the most likely explanation for these concentrations of brackish waters is localized remnant sea water that has become trapped.

Oceans are the largest single source of salts in the atmosphere, and chloride is one of the most abundant ions in air masses over the sea (Feth 1981). Chloride concentrations, therefore, is high in air masses near sea coasts. These airborne salts are delivered to coastal watersheds by precipitation and can increase in soils due to

111 evaporation and evapotranspiration. Chloride concentrations in precipitation, however, are relatively small compared to seawater.

It has been determined that there is often a correlation between distance from the coast and chloride concentrations in precipitation (Junge and Werby 1958). Chloride concentrations are high in air masses near sea coasts but decrease rapidly with increasing distance inland (Feth 1981; Davis et al. 2001), as these airborne salts can be delivered to coastal watersheds through precipitation. Previous studies have shown that concentrations of chloride in natural precipitation vary between less than 0.5 to more than

100 mg/L in North America. Davis et al. (1998, 2001, 2004) note that the CI/Br ratio can be traced through the hydrologic cycle from original values in seawater of 288, all the way through ratios in precipitation several hundred kilometers inland reaching values of

50 to 120. Davis et al. (2001, 2004) found that the natural mass ratio of CI/Br in precipitation varies in the United States from approximately 250 in coastal areas to approximately 50 in the northcentral U.S. states. Today, chloride in precipitation at

Roger's Brook, a site in central Nova Scotia, is 1.05 mg/L (Freedman and Clair 1987).

Chloride concentrations for precipitation data have been tabulated by the New

Brunswick Department of Environment (S. MacDougall, personal communication 2007).

The average concentration (mg/L) of chloride is derived by dividing the mass deposited by the amount of precipitation at 12 stations located throughout New Brunswick

(Figure 3.14) over a given period (usually annually). Chloride concentrations found in precipitation from seven of these locations are presented in Table 3.4. These sites follow the Saint John River from the Grand Lake Meadows region, in southcentral New

Brunswick, to the Bay of Fundy coast. The chloride concentrations in bulk precipitation,

112 St. Maure

Canterbury

Magaguadavic __ Lake V South OromoctdV Fundy National /Lake LonewateLonewat^V^r ^ Park ^^\f^W^^ Xakewood Heights Pennfield Musquash ^ NBDENV

igure 3.14: Location map where chloride concentration for precipitation data has been tabulated for twelve stations throughout New Brunswick by the New Brunswick Department of Environment.

113 Station In1 ormation Station Latitude Longitude Distance to coast Avg, chloride (km) (mg/L) Coals Island (Grand Lake Meadows) 45.9245 65.8107 64 0.4 South Oromocto Lake 45.4464 66.6492 58 0.6 Darlings Island 45.5019 65.8909 29 0.6 Lonewater Farm 45.3936 66.2450 22 0.7 Lakewood Heights (Saint John) 45.3128 65.9736 7 1.1 Musquash 45.1853 66.3325 5 1.6 Pennfield 45.1297 66.6575 5 1.4 Table 3.4: Chloride concentration (mg/L) from locations a ong the lower Saint John River. collected from all seven sites from the lower Saint John River valley over a number of years (4 to 18), exhibit a dependence on distance from the coast.

Maximum deposition of chloride occurs at coastal localities in New Brunswick, decreasing as the station locations move towards the interior of the province. Chloride deposition shows a decrease from the south to the central portion of the province, reflecting the greater importance of the marine air masses high in chloride closer to the coast, and the influence of air masses low in chloride in central New Brunswick.

Therefore, it has been determined that precipitation high in chloride due to distance from coastal marine water would have little effect on the chloride concentrations found in the

GLM-01 core.

A large portion of the GLM-01 sediment core has low CI/Br ratios with levels between 2.78 at 9 cm dbs and 117.39 at 48 m dbs, suggesting ratios similar to those that can be generated in brackish waters several hundred kilometers inland, well away from marine waters and the coastal margin. However, there are punctuated areas throughout the core that indicate deposition under more saline water conditions with a higher marine influence. These areas have CI/Br concentrations between 134.61 and 219.50. Even with

114 these higher CI/Br ratios, levels are still not indicative of seawater deposition with no freshwater influx.

Evidence for a marine transgression as ice left the lower Saint John River valley has been noted by marine deposits that mark the marine limit for the region between

~100 and 80 m above mean sea-level (Matthew 1872; Chalmers 1885, 1890; Golthwait

1912,1924; Kiewiet de Jonge 1951; Gadd 1973; Grant 1980; Rampton and Paradis

1981b; Seaman 1982; Rampton et al. 1984). Giudice and Broster (2006) interpret pockets of brackish water located throughout the lower Saint John River valley as remnants of trapped sea water from the DeGeer Sea inundation. Therefore, the most likely source of chloride and bromide found in the GLM-01 core is chloride and bromide remaining in the sediment from the marine transgression that followed the retreat of the

Late Wisconsinan ice sheet, some 13,000 years ago. Similar conclusions were also determined by Webb (1981), Guidice (2005), and Guidice and Broster (2006).

Davis et al. (1998, 2004) found that concentrations of chloride are typically very low around 0.003 to 0.06 mg/L in natural precipitation. It is also assumed that the chloride is sufficiently soluble that it only exists in the dissolved phase. However, chloride can be bound as precipitated salts in a caliche matrix that surrounds individual grains. Gillott (1968) suggests chloride does not constitute a large percentage in the mineralogical composition of clays and soils. As chloride is not commonly deposited in freshwater lakes, any measurable amount of chloride absorbed to the clay surface is often attributed to deposition in marine water. Gieskes et al. (1991) also suggest that very small, but distinguishable increases in dissolved chloride often attest to past salinity changes in the water.

115 3.4.7 Loss-on-Ignition

Percentages of LOI were used to indicate the presence of organics within samples obtained throughout the GLM-01 sediment core. LOI is a method that has been used by others in the region to measure the organic content of sediments for the delineation of past fluctuations in climate (Levesque et al. 1993b; Mayle and Cwynar 1995a). Using the percent of organics found in the GLM-01 core as representative of climatic conditions suggests that palaoclimatic conditions become warmer as the percentage of organics increases. However, it is important to consider that for the lower Saint John River valley organics would not only have come from terrestrial sources but would also have been introduced to the system through the inundation of post-glacial marine waters. Therefore, using samples from a closed system as opposed to an open system, such as found within the lower Saint John River valley, would potentially allow for a more unbiased conclusion when correlating climatic conditions with LOI.

It has been demonstrated that the \Vd550 weight represents ignition of all organic compounds in the sample (Dean 1974; Heiri et al. 2001; Smith 2003). However, few studies have considered the possibility of an LOI error due to the occurrence of coal in the sample (Malik and Scullion 1998; Marashi and Scullion 2003).

In the region around the GLM-01 drill site coal can be found in the local bedrock. These coal seams were sampled by Kalkreuth et al. (2000) to study vertical and lateral in-seam variations. It was determined that the range of thickness of the coal seams in and around the Grand Lake region was between 0.11 and 0.48 m, with an average thickness of 0.28 m.

116 Hand size to smaller pieces of coal can be found along the shores of the Saint

John River, Jemseg River and Grand Lake, and are thought to be anthropogenic in nature.

In 1639 a coal mine opened at Grand Lake and coal was shipped to Boston (http://dsp- psd.pwgsc.gc.ca/Collection/M39-78-2001E.pdf). This was just the beginning of coal being transported by boat down the local rivers.

Mining in Minto, ~50 km northeast of Fredericton on the north shore of Grand

Lake, began on a large scale during the late 19th century. During the early years of the

Great Depression, the New Brunswick Power Corporation built the province's first thermal generating station on the shores of Grand Lake, and it accessed coal from local deposits. Therefore, it was considered a possibility that any weight loss determinations in the LOI procedure may have been subject to error caused by volatilization of anthropogenic coal from the region (Figure 3.15).

Through archaeological excavations within the Grand Lake Meadows region fragments of coal identified macroscopically are often found in the upper one meter of sediment, likely due to historical transport of coal on barges down the Jemseg and Saint

John Rivers. Traces of black subangular fragments, thought to be possibly coal, were identified microscopically from seven sediment samples from throughout the core (Table

3.5). Samples from three locations were collected and further analyzed on the Scanning

Electron Microscope (Plate 3.11). The presence of coal was confirmed in one sample from a depth of 7.8 m dbs (C. Shaw, personal communication 2007).

117 Gulf of St. Lawrence

"X New / { i A / ~n A f <•* / < //Prince Edward

USA

* ^

^/•V^ Atlantic Ocean AtfA Mari times Coalfield Basin Figure 3.15: Location map depicting area in New Brunswick underlain by coal in the bedrock.

118 &m ;>^%^,

• 300|jm Plate 3.11: Coal was confirmed using the Scanning Electron Microscope in one sample from a depth of 7.8 m dbs (Cliff Shaw, personal communication 2007) (photo by P. Dickinson).

119 Depth (m) Coal fragments Coal fragments Coal identified identified collected with SEM 1.5 yes no no 7.8 yes yes yes 15.7 yes no no 23 yes no no 30.5 no no no 38.3 yes no no 45.8 no no no 53.5 no no no 59.8 yes yes no 62 yes yes no Table 3.5: Samples extracted from the GLM-01 core for coal identi :i cation.

Samples from known coal deposits from the region, Fire Road Mine and Salmon

Harbour Mine, located just north of the Grand Lake Meadows, near Minto, New

Brunswick, were collected and tested to ascertain local coal combustion temperature.

Laboratory tests were completed to establish if the coal would be burned off within the

550°C temperature used for LOI. If there were coal within the GLM-01 core the coal was thought to have come from one of these two local coal sources found within the

Carboniferous units of the area (Kalkreuth et al. 2000). The transport distance for coal detritus is dependent upon the hardness of the local coal variety (0.5 to 3.0 Moh's) and the energy of the transporting agent. In the Grand Lake region the coal is soft (<2.0

Moh's) and transport distance is likely limited to a few kilometers. Ignition tests on samples were conducted under various temperatures and duration to identify the optimum combination that would enable distinction between the organic and inorganic (coal) content by LOI.

The data from the first experiment determined the temperature at which the coal from the two coal mines was ignited. The tests indicated that at 300°C all the coal from both locations would be ignited (Figure 3.16). A more detailed thermographic analysis

120 1 UU/O

—•— Fire Road Test 1

80% - —•— Salmon Harbour Test 1

—*— Fire Road Test 2 w 60% - o *•> —*— Salmon Harbour Test 2 c 0) o £ 40% -

20% -

100 C 200 C 300 C 400 C 500 C Temperature (Celsius)

Figure 3.16: Summary of results depicting no significant difference in the temperature at which the coal from Salmon Harbour and Fire Road Mine ignited.

121 was carried out by Ramshaw (1985) in South Wales, increasing ignition temperatures in

10°C increments from 150 to 400°C. Ramshaw's (1985) study also confirmed that coal ignition began at 300°C and was largely complete at 340°C. Therefore, loss-on-ignition below 300°C provides a reasonable estimate of soil organic matter levels without the inclusion of coal. An additional analytical experiment using coal from the two different coal source samples from the Minto region was carried out to test the temperature and time to completely burn off each of the two coal samples (Figure 3.17). It was determined that the coal was completely burned off after -1.5 hours at 500°C.

Results indicate that initial ignition temperature of the coal from the Minto region was

~300° C, below the 550°C temperature recommended for organic LOI analysis. Testing indicated that time did not play a significant role in LOI, whereas temperature played a major role as sediment test samples stabilized after ~2 hours for all temperatures. Also, analysis indicated that organics other than coal burned off at 550° C after 2 hrs.

Hiemstra et al. (2007) identified coal in till sediments that was interpreted as representing zones of failure either at the till-bedrock interface or within the bedrock at depth. Therefore, to determine if the percent LOI in the till from the GLM-01 core may represent local coal found in the bedrock, black fragments from the till were examined macroscopically. These samples were placed in the SEM and coal was not identified

(C. Shaw, personal communication 2007). It is more likely that the record of LOI in the till is representative of primary or secondary pollen. Primary pollen has been found particularly in supraglacial tills or in the upper exposed portion of some till (Heinonen

1957), whereas secondary pollen has been entrained from pollen-bearing older sediments

122 LOI COAL BURNS

100%

~ 80% V) o 2- 60% c o

f 40% o •3 20%

0% 0 0.5 1.5 2 2.5 3.5 Time (hours)

Figure 3.17: Summary of results depicting that the coal from Salmon Harbour and Fire Road Mine were both completely burned off after ~1.5 hours at 500°C.

123 (Dreimanis et al. 1989). Dreimanis et al. (1989) suggest that tills that do not contain pollen probably consist entirely of freshly ground bedrock. Since coal was not identified in the till from the GLM-01 core it is possible that the results of the LOI completed on the till is representative of either primary or secondary pollen (Dreimanis et al. 1989).

Within the till the percent LOI was very low increasing to a high at ~53 m dbs where there is thought to be complete marine submergence in the lower river valley.

There are a number of fluctuations in the percent LOI throughout the core, with an average of ~3%, until there is a major drop at ~16 m dbs when Ancestral Grand Lake drains. At this point gravel is present in the core, the only gravel identified above the till.

Gravel continues in the core to a depth below surface of ~6 m. Throughout the gravel

LOI decreases to percentages similar to that identified in the till. The gravel is representative of faster flowing water, which would have winnowed out the fines and most of the organics that may have been present. At ~6 m dbs the gravel ends and sand begins. Here LOI continues to increase until it has reached a present day high.

3.5 Statistical Analysis

A description of the arrangement, dimension and nature of the sediment layers at the location of the GLM-01 core was used as a link to the spatial distribution of geologic processes for the region. However, explicit and quantitative models for the spatial prediction of soil and landscape attributes were completed to aid in landscape modelling.

In this study, advances in the spatial representation of hydrological and geomorphological processes using traditional soil lab analysis techniques (i.e. particle size analysis, atterberg limit determination and natural moisture content) are integrated with the

124 development of a sediment-landscape model-building strategy. Statistical models are developed (Spearman rank correlation, agglomerative hierarchical clustering and discriminant analysis) using relationships among grain size (gravel, sand, silt and clay), organics (loss-on-ignition) and mineral deposition (chloride and bromide) identified within the sediment core. These techniques provided an appropriate methodology for further development of sediment-landscape processes. Such a combination of techniques allowed for the spatial predictions of sediment layers, individual sediment attributes, and, eventually, sediment-landscape processes.

3.5.1 Spearman Rank Correlation

That two variables correlate can demonstrate a potential relationship; however, it does not demonstrate there is a definite relationship between the variables. Only through additional research is it shown that one variable affects the other. Analysis of loss-on- ignition indicates that within the Grand Lake Meadows basin organic carbon input has fluctuated since deglaciation; however, a scatter plot vs depth indicates that LOI has also experienced visible increasing trends at the lower and upper extremes of the core (Figure

3.18). There have also been a number of similar fluctuations in the chloride/bromide ratios throughout the core (Figure 3.19). The correlation of chloride and bromide with

LOI was found to have a strong positive correlation at the 99% level (0.23, n=123) (Table

3.6) when a Spearman Rank correlation was completed. The critical value for P(0.05) and P(0.01) suggest that the correlation between LOI and sand, silt, clay and percent silt plus clay is statistically significant (Table 3.6). However, the correlation coefficient for

125 Loss on Ignition (%) c) 1 2 3 4 5 6 7 8 9 0 -j rr^O • 10 -

.V^JJ>" 20 (S *^—*

^Wgj*—•

1 30 - Dept h

40 -

50 -

, wt • V***" J

60 -

Figure 3.18: Connected scatter plot of LOI.

126 CI/Br Ratio 50 100 150 200 250

10 A

& 30 a a> Q 40

Figure 3.19: Connected scatter plot of chloride/bromide ratio.

127 gravel is 0.12; therefore, the correlation of LOI and gravel is not significant at the 95% level.

LOI correlated with Correlation Coefficient (n=123) (r) Gravel 0.12 Sand 0.18 Silt 0.22 Clay 0.61 Percent silt plus clay 0.19 Chloride 0.41 Bromide 0.41 Table 3.6: Correlation between LOI and sand, silt, clay and percent silt plus clay, critical value 0.05 (0.17) and 0.01 (0.23).

The critical value for P(0.01) suggests that the correlation between chloride and bromide (0.70) is a strong positive correlation. A strong positive correlation was also noted between chloride and clay, and chloride and silt (Table 3.7). Additionally, a similar strong positive correlation was noted between bromide and clay, and bromide and silt

(Table 3.8).

Chloride correlated with Correlation Coefficient (n=123) (r) Gravel 0.09 Sand 0.15 Silt 0.25 Clay 0.35 Percent silt plus clay 0.20 Bromide 0.70 Table 3.7: Correlation between chloride and clay, and chloride and silt, critical value 0.05 (0.17) and 0.01 (0.23).

Bromide correlated with Correlation Coefficient (n=123) (r) Gravel 0.09 Sand 0.10 Silt 0.28 Clay 0.28 Percent silt plus clay 0.22 Table 3.8: Correlation between bromide and clay, and bromide and silt, critical value 0.05 (0.17) and 0.01 (0.23).

128 It is possible that some spurious correlations have been found when correlating grain size with LOI, chloride, bromide or with the chloride/bromide ratio. Such spurious correlations are due mostly to the influences of one or more "other" variables. For example, there is a correlation between the total amount of LOI and changes in grain size; however, what this correlation does not indicate is that these two variables (LOI and grain size) may actually be dependent on a third variable, regional hydrology. The initial size of the basin may also be a variable that influences both the amount of LOI and the grain size. The main problem with spurious correlations is that it is typically difficult to know what the "hidden" variable or variables are. Spurious correlations in geological research are not uncommon. It is very possible that they could occur when studying landscape processes, or when one variable represents a part of another variable. This could be particularly common when studying correlations within an open system, such as within the lower Saint John River valley, Grand Lake Meadows region.

Correlation, being a linear measure, cannot capture the non-linear relationships that may exist with most open systems. The trend for the LOI, chloride and bromide is linear; however, within the open system of the Grand Lake Meadows there have been a number of major short lived fluctuations in the LOI, chloride and bromide, and grain size.

These fluctuations within the system could relate to a number of factors such as deglaciation, climate change, isostatic adjustment, regional tectonic events, and anthropogenic influences. Therefore, the geomorphic diversity of an open system landscape, such as found in the lower Saint John River valley system, complicates correlation analysis.

129 3.5.2 Agglomerative Hierarchical Clustering

Agglomerative hierarchical clustering is a classification method that examines the similarities among samples, and groups similar samples in a hierarchical diagram at the levels of dissimilarity. Through cluster analysis it is possible to gain an understanding of a suitable number of classes into which the grouped data can be interpreted relative to causal relationships (i.e. facies, species, etc.).

Applying the single linkage method to the variables: depth, gravel, sand, silt, clay,

LOI, chloride and bromide, a Q-mode cluster analysis dendrogram was produced that classified the 126 observations for the sample population (Figure 3.20). Since the location of the research is within the center of an open landscape system, which allows for the transfer of both energy and matter to and from the system, a number of classes on the dendrogram were produced (Table 3.9).

Classes 1 2' 3 4 5 Objects 44 2 75 2 3 Table 3.9: Classes and object number produced on the dendrogram from the clustering analysis.

In studying the dendrogram three major facies were recognized (Figure 3.20), a fluvial facies, a deep-water marine/lacustrine facies and a till facies. The fluvial facies is defined as deposition associated with stream or river-related processes. Finer grains (silt and clay) have been picked up for transport in suspension and moved or deposited in a new location. The marine/lacustrine facies refers to an environment reflecting depositional mechanisms associated with the deposition of finer grains (i.e. silt and clay) rather than a facies associated with transportational mechanisms. Finally, the till facies is related to the deposition of unsorted sediment by glacial processes.

130 Figure 3.20: Dendrogram with eight variables (depth, gravel, sand, silt, clay, LOI, chloride and bromide). There are two "outlier" classes, which may relate to the geomorphology of the sedimentary environment as a whole. Just as the geomorphic diversity of the open system landscape complicated efforts to correlate variables, a similar complication could pertain to the agglomeration cluster analysis. Also, such an "outlier" may relate to likely overlaps between abutting profiles/environments of deposition. Therefore system distinctions may be inappropriate.

3.5.3 Discriminant Analysis

Discriminant analysis was used to check on a two-dimensional chart if the facies to which observations belong are distinct. To determine if five distinct facies could be distinguished, floodplain, fluvial, lake (brackish/lacustrine), marine and till (Figure 3.21), discriminant analysis was completed on observations relating to depth, grain size, LOI, chloride and bromide. The system classification had already been determined prior to the statistical analysis from examination of the variables with depth. Since the five distinct facies were already identified, it is not the aim of the discriminant analysis to create a new classification system, but to provide an unbiased statistical evaluation of the relevance of the five facies groupings.

For the discriminant analysis three quantitative observations relating to soil depositional environment, depth, chloride and bromide, were plotted against the five qualitative systems; floodplain, fluvial, lake, marine and till (Figure 3.22). Analysis suggests that the facies to which the observations belong are indeed statistically different from one another. The distinctions among the facies groups are also clear when the data are plotted with observations relating to hydrology and depositional environments, depth,

132 Floodplain

*r^^sr^s\^.*.^*\JrCy^l^ls^^^/\^^^^^s?'s

20 Lake

40 Marine

-Fig ure 3.21: Five distinct fades identified within the core.

133 Observations (axes F1 and F2:98.76 %)

x Floodplain a a A Fluvial % opa o •fc^D?1 CD o Lake lO a aft, CM a Marine ; o h +-*• • Till

iD D a • aa ani

-10 10 F1 (93.16 %)

Figure 3.22: Discriminant analysis with two quantitative observations relating to soil depositional environment (chloride and bromide) and depth, as plotted against five qualitative systems (floodplain, fluvial, lake, marine and deglacial till).

134 gravel, sand and percent clay plus silt (Figure 3.23). Finally, when depth, percent silt plus clay, LOI and CI/Br ratio are plotted, facies are also seen to be.distinct (Figure 3.24).

These results indicate that, in every case examined, allocation by discriminant functions agrees with the assigned five distinct facies as separate from one another.

135 Observations (axes F1 and F2:99.37 %)

x Floodplain

0s A Fluvial o Lake IT) ° Marine • Till

-5

-10 -10 10 F1 (93.43 %)

Figure 3.23: Discriminant analysis with three quantitative observations relating to hydrology and depositional environments (gravel, sand and percent silt plus clay) and depth, as plotted against five qualitative systems (floodplain, fluvial, lake, marine and deglacial till).

136 Observations (axes F1 and F2:97.47 %)

x Floodplain A Fluvial

CM ° Marine • Till

-5

-10 -10 10 F1 (87.33 %)

Figure 3.24: Discriminant analysis with four quantitative observations (depth, percent silt plus clay, LOI and chloride/bromide ratio), as plotted against five qualitative systems (floodplain, fluvial, lake, marine and deglacial till).

137 CHAPTER 4

RESULTS

The results of the analysis allowed for the development of a facies model of deposition to be constructed, which corresponds to the stratigraphy and interpreted stratigraphy (Figure 4.1) for the GLM-01 core.

4.1 Facies Model of Deposition

A facies model of deposition from the bottom to the top of the sedimentary sequence has been developed.

Facies: silty sand with pebbles and cobbles (~65 to 60 m dbs)

The silty sand with pebbles and cobbles facies is ~5 m thick and constitutes the basal unit in the core, just above the bedrock. The unit contains subangular pebble and cobble-sized clasts interspersed with coarse sand and silt, and are characterized by low

LOI (~1 %). The basal unit is interpreted to have been deposited during the early

Holocene deglaciation, which is consistent with other cores from the lower Saint John

River valley.

The texturally variable loose, non-compact, permeable subangular pebble and cobble-sized clasts interspersed with coarse silty sand is indicative of till, possibly related to ablation till, which would suggest melt-out of englacial material over bedrock.

Facies: stratified silty sand; silt; silt with sand; sandy silt and silty clay (-60 to 56 m dbs)

This facies is located just above the till. The unit is ~4 m thick, dominated by stratified silt and sand with a minor admixture of clay. The water content increased from

138 Modern alluvial floodplain: SILT, SILT with sand, and sandy SILT

Fluvial outwash: Interbedded poorly graded SAND with silt, poorly graded 10 1 sand, and silty SAND

Upper ponded environment: SILT, SILT with sand, and sandy SILT 20 m Silty SAND

••£ 30 -I

Q. Q Upper ponded environment: SILT, SILT with sand, and sandy SILT

60 4 Glacial till: silty sand with pebbles and cobbles 'I I I I I I I I I I I I I I I II I I I I I I I I I I I I I I I I I I I I I I I I IT Figure 4.1: Facies model of deposition depicting the stratigraphy and interpreted stratigraphy for the GLM-01 core. the bottom to top of unit from 21 to 35%, with the grain size, LOI and CI/Br ratios all following a similar trend (Figure 4.2). However, the bromide was below the detection limit or <0.5 mg/L in two core locations, just above the bedrock from 59.02 to 58.21 m dbs and at 56.74 m dbs. This low to undetectable bromide content is indicative of areas of deposition under conditions where there was an influx of large quantities of fresh glacial melt-water into a marine/brackish environment. During periods of high glacial melting the bromide content became completely diluted by an influx of freshwater.

This unit is a complex stratigraphic succession interpreted as being associated with ice recession and ponding. From bottom to top the unit consists of interbedded sediments possibly representing a former outwash plain and proglacial lake materials.

This unit was interpreted as an early ponded environment material, representative of minor standstills and ice front oscillations during the early Holocene deglaciation. The unit was deposited in front of a receding ice margin as marine and freshwater were both in contact with the ice.

Facies: silt; silt with sand and sandy silt (-56 to 15 m dbs)

This is a heavily laminated facies ~41 m thick. The number of laminae per

610 mm fluctuates from a high of 187 to no laminae present closer to the top of the facies. Vivianite and shell fragments are present only in this facies, from 42 to 16 m dbs.

Wood organics become present in the sediment at 42 m dbs and continue throughout the core to the surface.

This facies is characterized by a fairly stable water content averaging 33.7% with a range of 27 to 46%. The Atterberg limits start to increase at the bottom of the facies

140 a) b) c) d) e)

Stratigraphy Age BP (years) CI/Br Ratio Loss on Ignition ("/^ Grain Size (Cummulative %) 0 10000 0 200 400 0 5 10 0 20 40 60 80 100

• = •

•

HM*KKKKi - SILT + CLAY'

Figure 4.2: Summary of results of laboratory testing of core, a) stratigraphy, b) AMS radiocarbon dates, c) chloride/bromide ratio, d) loss-on-ignition and e) grain size.

141 from 21 at 57 m dbs to 41 at 53 m dbs, where it then drops very gradually to 24 at 24 m dbs. The LOI trend is fairly consistent, slightly decreasing from bottom to top averaging

3% with many small fluctuations. This trend follows in the CI/Br ratio, averaging 104 with a decreasing ratio from bottom to top. The oldest AMS date of 11,340 ±210 was obtained on a wood fragment from 28 m dbs. Four additional AMS dates, with the youngest date of 7770 ±80 at 16 m dbs, were obtained from this facies (8150 ±80 at 25 m dbs, 9600 ±22 m dbs and 7820 ±90 at 19 m dbs).

This facies constitutes most of the middle portion of the core and represents an upper ponded environment with slow sedimentation of fine-grained material, chloride and bromide, as well as organics. The fluctuations in the percent LOI and grain size are interpreted as reflecting short-term climatic changes. Additionally, the fluctuations in the

CI/Br ratio and grain size may also reflect changes in hydrology. This could be controlled by isostatic adjustment and the expansion and melting of local glaciers in the catchment area allowing for more or less saline water of varying depths into the region.

Facies: interbedded poorly graded sand with silt; poorly graded sand, silty sand and gravel (~15 to 3 m dbs)

This ~12 m thick facies has been identified just below the modern fluvial sediments. No vivianite or shell fragments were found; however, some wood fragments were identified. The unit is characterized by a moisture content that is very similar to the facies below, having an average of 31 %. The trend for the LOI and CI/Br ratios are - similar, with a decrease in organics, chloride and bromide. The percent LOI between 15 and 7 m dbs is generally lower than the preceding facies, with an average of ~1.5%. The percent of LOI increases from 7 to 3 m dbs from 1 to 3% respectively. There is no CI/Br

142 ratio for this fades as the bromide was <0.05 to undetectable, representing freshwater deposition. Three AMS dates from this facies were obtained on wood fragments. The

AMS dates were consistently younger as depth decreased from 4770 ±70 at 12 m dbs,

3820 ±60 at 10 m dbs, and 3080 ±70 at 6 m dbs.

This upper sand and gravel-bearing facies is interpreted as fast-flowing fluvial outwash representing an active channel. Hydrology has increased as seen by the winnowing out of the fines. The lack of stratification points to highly concentrated, non- tractional mass flow of water.

Facies: silt; silt with sand and sandy silt (~3 m dbs to surface)

The silt, silt with sand and sandy silt facies is found at the surface and is ~3 m thick. It rests on the coarse-grained fluvial outwash material. No lamination of the sediment is present. The facies is characterized by a water content averaging 33.5%, similar to the previous two facies. The LOI trend increases towards the surface from

~2 to 6% with an average of 3%. The CI/Br ratios fluctuate in this top 3 m, ranging from

~3 to 70, with an average of 25. One AMS date of 110.36 ±0.70 was obtained on a wood fragment from 71 cm dbs.

This sharp bounded layer consists of chloride and bromide, which was not present in the previous facies. The LOI increased from an average of- 2 to 3% from the previous facies reaching 6% at 30 cm below the surface. There was also an increase in the percent of fines (silt and clay) with an average of-18% in the previous facies to an average of-73% in this facies. This surface facies is interpreted as modern alluvial floodplain material.

143 4.2 Stratigraphic Units

The stratigraphic units within the GLM-01 core (Figure 4.1) are consistent with the stratigraphic units found in the transect of cores crossing the Saint John River and

Jemseg River (Figure 3.2) in the Grand Lake Meadows region. The individual thicknesses of the five unconsolidated units are also similar. The validity of the stratigraphic interpretation is strongly supported by additional laboratory data, which show that the stratigraphic changes coincide with marked changes in grain size distribution, loss-on-ignition, and chloride and bromide concentrations. The interpreted stratigraphies of the unconsolidated units are, from bottom to top: bedrock, till, early ponded environment, upper ponded environment, fluvial outwash and modern fluvial floodplain (Table 4.1).

Depth Below Stratigraphy Interpreted Stratigraphy Surface (m) Surface —3 Silt, silt with sand, sandy silt Modern fluvial floodplain -3-15 Interbedded poorly graded sand with silt, Fluvial outwash poorly graded sand, silty sand and gravel -15-56 Laminated silty sand Upper ponded environment -56 - 60 Silty clay Early ponded environment -60 - 65 Pebbles and cobbles with coarse sand, Till silt and clay -65 m Consolidated rock Bedrock Table 4.1: Stratigraphy and interpreted stratigraphy produced from the GLM-01 core.

The bedrock is the lowest unit found just below the depositional retreat sequence in the Grand Lake Meadows. As discussed in more detail in Chapter 1, the area is underlain by Carboniferous sandstone and conglomerates (Clark 1962; Gadd 1973;

Ferguson and Fyffe 1985).

Glacial till has been deposited directly on top of the bedrock. The till from within the GLM-01 core may be related to ablation till due to the material being identified as

144 loose, permeable material consisting of crudely sorted pebbles and cobbles with coarse sand, silt and clay matrix. The thickness of the till from the GLM-01 was ~5 m. Till from the Saint John River bridge crossing cores were <5 to 25 m in thickness, thickening away from the center of the palaeochannel, whereas till from the Jemseg River bridge crossing cores were <5 m in thickness across the entire channel.

The early ponded environment is interpreted to be represented by material deposited by slow moving to ponded glacial melt-water and consist of laminated (from bottom to top): silty sand; silt, silt with sand and sandy silt; silty sand; silt, silt with sand and sandy silt; and finally silty clay. Together these sediments had a thickness of ~5 m.

The early ponded material from the Saint John River bridge crossing cores were <5 m thick in the deepest portion of the palaeochannel and ~1.5 m thick furthest away from the center of the palaeochannel. The early ponded sediment from the Jemseg River bridge crossing cores were <5 m in thickness furthest away from the center of the palaeochannel with no deposit present in the center of the channel. The cores from the two river crossings suggest that the early ponded sediment was eroded by a high-energy glaciofluvial event. The early ponded environment is interpreted to represent mainly a glaciomarine environment on the basis of the CI/Br ratios.

The upper ponded environment consists of a laminated, primarily silt, silt with sand, and sandy silt unit and has been interpreted to be deposits from a brackish water environment. This unit from the GLM-01 core was ~40 m thick. Similar units with a similar thickness of ~45 m were identified in the Saint John River bridge crossing cores pinching out closer to the surface, away from the center of the palaeochannel. Similar sediments were also identified in the Jemseg River bridge crossing cores; however, they

145 were identified as ~20 thick but also pinching out away from the center of the palaeochannel..

A postglacial fluvial outwash unit was identified as poorly graded sand with silt, poorly graded sand, silty sand and gravel. This fluvial unit is -12 m thick. A similar unit, with a similar thickness of 10 m, was identified in the Saint John River bridge crossing cores. This unit was slightly thicker in the Jemseg River bridge cores at 10 to

15 m.

The identified modern fluvial unit includes silt, silt with sand, and sandy silt.

This ~3 m thick unit, extending to surface, has been interpreted as modern river floodplain deposits. This surface unit was ~10 m thick in the Saint John River bridge cores and pinched out away from the center of the palaeochannel. This same unit was just less than 10 m thick in the Jemseg River bridge cores.

The interpreted unconsolidated stratigraphy for the sediments at Fredericton

(Daigle 2005), from bottom to top consisted of: bedrock, ice-contact, lodgement till, ablation till, ice contact, till, ice contact, glaciofluvial, ponded environment, glaciofluvial and post-glacial. The stratigraphy for the Waasis borehole BH-1 was similar except the glaciofluvial sand and gravel unit between the till and clay/silt units was absent (Guidice

2005). The stratigraphy for the GLM-01 borehole was different than that found in the

Fredericton core by Daigle (2005) in that the pre-glacial sand and gravel unit identified below the till was absent. Additionally, the GLM-01 core had only one till present and no ice contact material. It was found that an early ponded environment material was deposited on top of the till with no glaciofluvial material between.

146 There are a number of possible interpretations relating to the units not found in the GLM-01 core. It is possible that some of the early units, below approximately 56 m dbs, were eroded by either a high-energy glaciofluvial event or reflect non-deposition Or a hiatus of some of the sedimentary units. The GLM-01 core was located in a very deep, wide basin within the lower Saint John River. Therefore, it is possible that there may have been substantial erosion of the till, ice contact and early glaciofluvial material postglaciation. Different thicknesses were identified of individual units across the channel in the lower stratigraphic units from the Saint John River bridge and Jemseg River bridge crossing cores. This may be suggestive of differential erosion in different portions of the palaeochannel with the greatest erosion found in the center of the channel.

Additionally, the Grand Lake Meadows may have been an area of extending ice calving. As the retreating ice was in constant contact with the seawater the depth of the water would have continued to increase in the Grand Lake Meadows region. This deepening water would have initiated a rapid calving retreat of the ice margin inland away from the Grand Lake Meadows. As the water in front of the glacier grew in size and deepened this would have allowed for the calving process to become more efficient in the area. With such rapid calving there would have been no stationary ice in the region, no grounding line, and therefore no ice contact material deposited, resulting in a hiatus in ice contact material deposition.

147 CHAPTER 5

DISCUSSION

Regionally, the lower Saint John River valley, its floodplain and adjoining tributaries, are the conduits through which the Saint John River basin's runoff and sediment load passes or is trapped. Additionally, the richness of the cultural resources found in the valley system indicates that this region was an attractive settlement location, in the present as well as the past. These factors in combination mean that the valley and floodplain environment contains a rich record of both past environments and past human occupation.

Reading the record of its past is not easy, however. From a palaeoenvironmental perspective, the relationship between alluvial deposits and the environmental changes they signify is complex. Such complexity is similar from an archaeological perspective, as the highly dynamic environment of the valley system has led to changes in settlement pattern and post-depositional modification of the archaeological record. An understanding of these complexities is essential when making an effort to understand the stratigraphy and glacial history of the region, as well as improving archaeological reconstructions, sampling and recovery. Clearly, the research challenge relating to environmental and landscape reconstructions and cultural resource management can, and should, be linked.

The study of late Wisconsinan and Holocene geology can provide a critical link between archaeology and landscape reconstruction. Long-term sedimentary records, such as found in sediment cores, give insight into landscape elements and change.

148 Palaeolandscape studies can answer questions relating to past environments as well as lead to inferences related to future landscape change. On both large and small scales the systems being studied are recorded in the sedimentary record.

This study has demonstrated the potential of a methodological approach designed to distinguish changes in local lacustrine and marine depositional environments. Such a methodology is particularly useful for the reconstruction of past fluvial histories.

Additionally, this methodology provided detailed information about the Holocene evolution of the lower Saint John River valley allowing for the archaeology of the region to be placed into a broader topographic and environmental context.

Using the stratigraphic information discussed here, it is possible to develop a landscape reconstruction for the lower Saint John River valley and to delineate palaeolandscape controls since the Wisconsinan deglaciation. Additionally, it is anticipated that the information generated from the data could be used by archaeologists and archaeological regulating bodies to place archaeological research and cultural resource management pertaining to the lower Saint John River valley and Grand Lake

Meadows region into a wider context.

5.1 Glacial History

The nature of the local unconsolidated sediments within the study area was identified by delineating the underlying stratigraphy of the sediments extracted from the

GLM-01 core. The stratigraphy consists of bedrock overlain by a glacial retreat sequence.

149 Approximately 14,000 BP ice sheets over the eastern coastal region of New

Brunswick started to retreat, leading to a number of events and geomorphological impacts:

1. development of the DeGeer Sea;

2. complete marine submergence of exposed land in the southern and eastern

portion of the province;

3. possibly early isostatic rebound of the eastern portion of the province cutting

off saline influence from the east;

4. isostatic rebound and the possible migration of a forebulge across the southern

portion of the province cutting off saline influence from the south;

5. development of Ancestral Grand Lake in the region of the Grand Lake

Meadows, impounded by the migrating forebulge and isostatic rebound in the

south;

6. draining of Ancestral Grand Lake due to migration of the forebulge through

the region and isostatic rebound in the central and northern portion of the

province, beginning of a fluvial environment;

7. breaching of saline water into the lower Saint John River at the mouth, over

the Reversing Falls, the beginning of an estuarine environment; and

8. development of the modern lower Saint John River valley and Grand Lake

Meadows.

The oldest radiocarbon date obtained from the GLM-01 core was from 28.6 m dbs at 11,340 ±210 years BP (TO-13071), which suggests that complete marine submergence lasted until isostatic rebound and the presence of a glacial forebulge blocked any contact

150 to marine waters. Complete marine submergence of saline water was indicated as occurring at -12,700 BP by Rampton and Paradis (1981b) and -13,000 BP by Nicks

(1988). This would suggest that early post-glacial marine submergence occurred within the lower Saint John River valley for a minimum of-2000 years. Additionally, if the impoundment of Ancestral Grand Lake, which started as a glacier-fed lake, occurred

-11,500 BP and it met its demise at -8000 BP then this lake existed in the lower Saint

John River for -3500 years. This indicates that the lower Saint John River valley was covered by marine/brackish water for -5000 years after the glaciers retreated from the region depositing a thick sequence of marine to freshwater sediments over the Grand

Lake Meadows area.

The lower Saint John River valley was open to saline water as the ice front was retreating from the region. The water changed from being saline, brackish, to eventually more fresh, with the later development of Ancestral Grand Lake. The Grand Lake area today developed from what was probably a saline stratified freshwater lake, similar to the stratification we see today in the region between Reversing Falls and the Kennebecasis sill (NB Power 2002, p. 10). The early marine incursion and later brackish and freshwater lake were synonymous throughout the region making it potentially difficult to separate marine and lacustrine deposits in the lower river valley. However, distinctions between marine and freshwater deposits can be determined in more restricted or narrow tributary valleys of the Saint John River, such as the Oromocto River valley, where there was little to no saline influence (Giudice 2005).

151 5.2 Climate Determined from LOI Analysis

The Grand Lake Meadows region was ice free and vegetated well before ~11,340

BP. Loss-on-ignition tests indicate that the basin has received significant organic input since deglaciation. The organics are interpreted as pollen and organic remains deposited in an open (uncovered) body of water. It is probable that the basin has received significant levels of both marine and terrestrial organic residue. Therefore, the LOI reflects more than just terrestrial plant colonization of the area since deglaciation, but also represents trapped pelagic organics as well.

The LOI analysis from the GLM-01 core is not wholly reflective of climate change within the lower Saint John River valley post glaciation. The percent LOI for the portion of the core between ~16 and 6 m dbs is comparable to that found in the till. Such a low percent LOI is likely the result of the increased grain size of the sediments found in this portion of the core. The increased grain size suggests a high water velocity, ultimately winnowing out the organics with the fines. Therefore, LOI analysis from an open system may not only change as climate and vegetation changes, but also as grain size and hydrology changes.

The LOI analysis from the GLM-01 core does indicate that organic production did continue from deglaciation until present day. This suggests that glacial ice did not cover the Grand Lake Meadows region during the Younger Dryas. The oldest date obtained on organics from the core was 11,340 ±210 years BP (TO-13071) at approximately 29 m dbs. From -53 to 15 m dbs, which returned an AMS date of 7770 ±80 years BP (TO-

13067), the percent LOI was fairly consistent with no drop in LOI lasting any extended period of time. There was a slight decrease in LOI at 26 m dbs that may be

152 representative of the Younger Dryas and is suggestive of low organic production, but not a complete cover of ice in the region.

5.3 Prehistory and Human Habitation

The landscape of the lower Saint John River valley offers some of the most attractive environments for human activity and settlement. This region has been attractive throughout the Holocene for its extensive transportation networks, settlement locations and the potential for resource exploitation. Today, development such as road, pipeline and housing construction, clearly poses a threat to widespread multi-period archaeology that has developed over late glacial deposits. Additional anthropogenic threats to cultural resources include: aggregate extraction, agricultural ploughing, peat extraction, road and building construction and drainage works.

Palaeoenvironmental reconstructions have been conducted in the adjoining state of Maine that illustrate environmental and landscape changes throughout the Holocene from open lakes to marshes (Sanger and Newsom 2000). Additionally, Almquist-

Jacobson and Sanger (1999) suggest that key resource procurement areas changed through time from lakes, to marshes, to peatlands, while significant upland vegetation species underwent variability in terms of species mix (Almquist-Jacobson and Sanger

1995). An understanding of the change in the spatial structure of landscape elements and their change through time, as illustrated in the following four depositional phases for the lower Saint John River valley, is key to understanding the regional distribution of cultural resources. Deciphering the positional status of cultural resources within the landscape

153 requires knowledge of the dominant environments and processes that have affected that

landscape through time.

It is important to reconstruct the landscape that existed around an archaeological

site or group of sites at the time of occupation. Crumley and Marquardt (1990) defined a

landscape as relating to the spatial manifestation of the relations between humans and

their environment. This is important because reconstructions of past human behaviour

are incomplete unless a site is placed in its non-cultural environmental context. Regional

and local geology influenced such things as fresh and marine water, human resource

procurement, as well as, site formation and preservation. The geomorphic landscape is a

dynamic component of the environment in which all biological organisms have lived and

interacted. Therefore prehistoric human occupation of the lower Saint John River valley

. must be placed in the context of its dynamic and evolving landscape. To gain an

understanding of the relationship people had with the land it is essential to reconstruct

both the dynamic and constant elements of that landscape, and recognize that it may not

have corresponded to the configuration of the existing one.

This project was proposed and undertaken to provide detailed information about

the Wisconsinan-Holocene evolution of the lower Saint John River valley, in order to

place the cultural resources of the floodplain into a broader topographic and

environmental context. An objective of this study was to delineate the relationship

between the palaeo-landscapes and occupation of the lower Saint John River valley by

pre-contact people. The Wisconsinan-Holocene geological history of the lower Saint

John River valley may now be used as a framework for known archaeological events, as

154 well as a general basis for archaeological predictive modelling of precontact site locations through time.

We know that the early DeGeer Sea covered was covering the lower Saint John

River valley -11,500 BP. These deep marine/brackish waters inundated the region for

~1500 years. The saline waters from DeGeer Sea were blocked off -11,500 BP and the stratified Ancestral Grand Lake developed in the lower Saint John River valley, lasting until ~8000 BP. Salinity levels would have been graduated vertically in the impounded lake, representative of a halocline. Since the presence of salts increases density, the lighter freshwater would have remained at the surface, while the salinity would have been greater at depth. People could have lived along the margins of the DeGeer Sea and

Ancestral Grand Lake for -5000 years. Such sites would be located on strandlines and deltas found between ~100 and 80 m asl and the present shoreline. As there are a number of terraces found at decreasing elevations within the lower Saint John River valley this suggests a slow, gradual increase and/or decrease of the elevation of water, at times maintaining a specific elevation marked by the development of beach-like terraces.

It is possible that people were living in the lower Saint John River valley region along the shores of the glacial lake even during the Younger Dryas cold period.

However, if there was a readvance of an isolated ice cap from the Caledonian Highlands during the Younger Dryas, LOI analysis suggests that this ice readvance did not cover the

Grand Lake Meadows region.

Between -8000 and 3000 BP there was a lowering of sea-level (base level) and the Bay of Fundy was dry except for a possibly braided or meandering river system out to the Scotian Shelf. At this time the lower Saint John River and Grand Lake Meadows

155 consisted of a major fluvial system represented by an increase in grain size and a decrease in chloride, bromide and LOI. This was the beginning of the modern Grand

Lake Meadows. Cultural resources within the river valley representing locations of human habitation at this time may now be under water or at the shores of the current

Saint John River or Grand Lake Meadows. Sometime after -3000 BP saline water was again introduced to the lower Saint John River system as marine water from the Bay of

Fundy breaches the Reversing Falls. A slow submergence of the Bay of Fundy coast, an increase in tidal amplitude along with a rise in sea-level, which has continued at a slow rate until present, has resulted in the drowning of the lower Saint John River valley producing the modern floodplain and estuarine environment visible today. The increased water level since ~3000 BP along with the annual flooding of the lower river valley would have completely flooded or seasonally flooded many cultural resources in the valley bottom.

All archaeological sites are not contemporaneous and the environment is not a static entity. As the environment is ever changing it is important to consider how, when and why it changed. An understanding of the landscape and landscape change through time will benefit research perspectives relating to archaeological site location, function and landscape context, as well as, allow the environmental context of archaeological periods to be elucidated.

156 CHAPTER 6

CONCLUSIONS

I have focused on developing and refining a local chronological sequence for the changing landscape and subsequent human occupation of the lower Saint John River valley. From this geological framework it is possible to predict past implications for human habitation within the river valley, as well as to the Grand Lake Meadows marshland.

6.1 Post Glacial Geological Interpretations of the Grand Lake Meadows Region

Analysis of the sediment from the GLM-01 core revealed four phases of deposition within the lower Saint John River valley since the end of the Wisconsinan glaciation. The four depositional phases establish the presence of a dynamic system within the river valley depicting landscape and environmental change.

The four phases of the lower Saint John River basin development can be tied to absolute dates and set a chronological framework for the development of the Grand Lake

Meadows. When the dates are arranged in a temporal sequence, they reveal dated stratigraphic units between 11,340 ±210 years BP (TO-13071) at 28 m dbs and 110 ±70 years BP (TO-13063) at 0.7 m dbs. The AMS dates obtained from the core were useful in providing actual age estimates for events and providing minimum constraints. The oldest date was obtained from organics found in the mid-section of the sediment core.

Another ~30 m of sediment, varying in LOI, chloride and bromide content, and grain size, was deposited below this dated organic material. Therefore, the date of 11,340 ±210

157 years BP (TO-13 071) does not reflect the maximum possible age of the sedimentary units at this location.

Phase I: Deglaciation in a marine environment to ~11.500 BP

Just prior to the Holocene there was a climatic warming and the commencement of a woodland environment with a rise in spruce and oak, poplar, cedar and juniper

(Mayle and Cwynar 1995a). The oldest reliable date from lacustrine deposits is 12,000

BP based on AMS dating of terrestrial plant macro fossils from Mayflower Lake near

Saint John (Mayle et al. 1993a, 1993b). An AMS date extracted from 28 m dbs on a wood fragment from the GLM-01 core, along with the percent LOI, suggests that the southcentral portion of the province at the Grand Lake Meadows was ice free by at least

11,340 ±210 years BP (TO-13071). However, a wood fragment too small to date was also extracted from the sediment core at -41 m dbs, suggesting that the region was ice free prior to this date. This wood fragment was determined to be in situ as it was bounded on the top and bottom by undisturbed laminae.

Salinity was a key factor affecting the physical makeup of the lower Saint John

River valley for most of its history. The early salinity levels would have varied, depending on sea-level and the volume of freshwater that was flowing off the melting glaciers and down deglaciated tributaries. Salinity would have declined during warm periods as melting ice would cause large increases of freshwater inflow pushing more saline water away from the front of the glacier. During colder periods, if ice were still in the region, freshwater inflow would have been reduced, resulting in high levels of salinity extending further inland, closer to the glacier front and possibly up some ice free tributaries.

158 The early DeGeer Sea, which covered southcentral New Brunswick, may correlate with the Goldthwait Sea marine incursion that affected areas of the St.

Lawrence Lowland (Gadd 1988) and western Newfoundland (Elson 1969). Within the

GLM-01 core, from -62 to 53 m dbs, the LOI and CI/Br ratio both begin to increase in a linear fashion. The LOI increases from ~1 to 4% and the CI/Br ratio increases from

-13 to 219. At the same time the grain size decreases from a sand rich to clay rich sediment. The decrease in grain size and following increase in CI/Br ratios indicate the early development of a marine incursion over the region by the DeGeer Sea (Rampton et al. 1984). The record of LOI in the till (<1%) probably does not indicate the inclusion of concentrations of coal fragments originating from the brecciated substrate, as coal was not identified in the till sample. The LOI in the till probably suggests the inclusion of secondary pollen that was entrained from pollen-bearing older sediments (Dreimanis et al. 1989).

At -53 m dbs the CI/Br ratios, clay content and LOI reach some of the highest levels attained throughout the core. The increase in LOI at -53 m dbs may represent significant pelagic input of organics with the post glacial marine incursion and development of the DeGeer Sea (Rampton et al. 1984). The later LOI above -53 m dbs may be more representive of terrestrial organic input.

As depth below the surface decreases, LOI fluctuates with a slight linear decrease.

There is a similar trend in the fluctuations of the CI/Br ratios with a decrease in a linear fashion as depth below surface decreases. At the same time grain size increases from a clay-rich to silt/sand-rich sediment. If the early DeGeer Sea correlates with the

Goldthwait Sea marine incursion, an early fluctuation in the CI/Br ratio may represent

159 isostatic rebound and the demise of a marine influence from the east/northeast. The lower St. Lawrence region lies on the south shore of the St. Lawrence estuary. The landscape is characterized by lowlands bordering the river. At 14,500 BP, approximately

1000 years earlier than the southern portion of the province, the ice sheet covering this region began to gradually melt as the climate became warmer. This may have allowed for isostatic rebound to occur earlier in the eastern portion of the province.

Complete submergence by marine water was indicated as occurring at -12,700

BP (Rampton and Paradis 1981b) and prior to -11,500 BP in the GLM-01 core. This would suggest that early postglacial contact with the sea and marine submergence of the lower Saint John River valley, due to glacio-isostatic depression, occurred within the lower Saint John River valley for a minimum of 1500 years.

Phase I represents a marine incursion over the region and the gradual desalinization of water due to pulses of freshwater from melting ice and retreating glaciers. This phase is undated in the GLM-01 core; however, it is represented by the lower 50% of the sediment core.

Phase II: ~11.500 to 8000 BP

A number of studies have clearly documented the presence of a cool interval in

New Brunswick between 10,770 and 10,000 BP that can be correlated with the Younger

Dryas Chronozone from northwestern Europe and the North Atlantic Ocean (Rawlence

1988; Rawlence and Senior 1988; Levesque et al. 1993a, 1993b, 1994, 1996, 1997;

Mayle et al. 1993a, 1993b; Cwynar et al. 1994; Mayle and Cwynar 1995a, 1995b). Just prior to the Younger Dryas there was a brief cold period called the Killarney Oscillation lasting from 11,160 to 10,910 BP (Levesque et al. 1993b). These events may be

160 represented in the GLM-01 core at ~26 m dbs by an increase in the CI/Br ratio, an increase in grain size, and a decrease in the percent of LOI. The CI/Br ratio throughout the core fluctuates from highs of 168 to lows of 9. These fluctuations possibly reflect freshwater pulses from melting ice to the north, as ice was present in the upper Saint John

River valley until 10,000 BP (Kite and Stuckenrath 1989). These pulses of water are also illustrated by fluctuations in grain size representing changing hydrology.

During the onset of these cold events (Levesque 1989) there was a change in the vegetation with a drop in spruce and the disappearance of oak, cedar and juniper trees, coinciding with an increase in shrub tundra vegetation such as alder, willow and sedge

(Mayle and Cwynar 1995a). Mayle et al. (1993a, 1993b) suggest that a drop in organic content would not only result from a decline in the deposition of organic matter, but also relate to an increase in the deposition of inorganic matter. Influx analysis confirms the notion that the relative decline in organic content is related to an absolute increase in the deposition of mineral matter indicating an increase in erosion at this time (Mayle et al.

1993a, 1993b). Cwynar et al. (1994) also suggest there was a great influx of inorganic material during the Younger Dryas, which relates the decline in organic matter with an increased erosion rate. This increase in erosion during the Killarney Oscillation and

Younger Dryas cold periods is correlated with the increased grain size from the GLM-01 core found between 27 and 25 m dbs. At the end of the Younger Dryas organic content of the sediment rises abruptly and the influx of inorganic matter declined (Cwynar et al.

1994). There is a decline in grain size in the GLM-01 core at the end of the Younger

Dryas (-25 m dbs), which also indicates a decline in the influx of inorganic matter.

161 Foisy and Prichonnet (1991) suggested that a residual ice cap (Gaspereau Ice

Centre) overlay the Caledonian Highlands at the end of the Late Wisconsinan, and

Seaman (1988a, 2006) postulated that this ice cap was also in place and expanding during the Younger Dryas. Seaman (2006) agrees with the north and west margin of the

Gaspereau Ice Centre during the Younger Dryas proposed by Lamothe (1992); however, he suggests that the southern margin was probably continuous across the southern part of the New Brunswick Lowlands, extending into the Grand Lake basin.

As indicated by the LOI analysis from this project it appears that glacial ice did not cover the Grand Lake Meadows region during the Younger Dryas. The oldest date obtained on organics from the GLM-01 core was 11,340 ±210 years BP (TO-13071) at approximately 29 m dbs. From -53 to 16 m dbs (-7770 BP) LOI was fairly consistent with no drop lasting any extended period of time. There was a slight decrease in LOI at

26 m dbs that may be representative of the Younger Dryas, suggesting low organic production, but not a complete cover of ice in the region. The largest drops in LOI are at

-60 m dbs just at the beginning of deglaciation, and between 16 m (-7770 BP) and 6 m dbs (-3080 BP), well before and well after the Younger Dryas.

Between -28 and 16 m dbs fluctuations and a drop in the CI/Br ratios may represent differentiated rebound in the south and/or the migration of a postglacial forebulge across the region. These fluctuations imply a declining marine influence in the region, and the development and demise of Ancestral Grand Lake. The earth's lithosphere is initially depressed by the thick glacial ice sheet. The weight of the glacial ice pushes down on the earth's crust causing the earth's mantle to be pushed up into a

162 bulge adjacent to the ice front. As the mantle material is viscous, the forebulge relaxes slowly and maintains its shape as it moves inland upon deglaciation.

Barnhardt et al. (1995) suggest the migration of a forebulge of-25 m in amplitude moved across the Maine coast at 10,500 BP. It was further recognized by

Dionne (1988) that the crest of the forebulge passed Quebec City -6500 BP, approximately 4000 years later than across the Maine coast. Balco et al. (1998) investigated the lake-level history of Moosehead Lake in northwestern Maine, and suggested that the lake basin was tilted to the northwest at 10,000 BP. By -8750 BP there was a relaxation of the landscape in Maine and the basin tilted to its current southeast position, possibly due to the migrating isostatic forebulge. Interpretation of the

GLM-01 core suggests that the forebulge could have also passed through the Grand Lake

Meadows region allowing for the development and later release of Ancestral Grand Lake

-8000 BP. Moosehead Lake is very close to Grand Lake latitudinally. Therefore, the migrating forebulge across Maine and New Brunswick may have occurred at a similar time. In New Brunswick the forebulge may have blocked any marine influence from the south at -11,000 BP allowing for the development of Ancestral Grand Lake in the lower

Saint John River valley and later released any trapped water at - 8000 BP. This lake would have been a predominantly freshwater lake; however, likely stratified with brackish water in the deeper parts of the basin. The initial development of Ancestral

Grand Lake would have been synonymous with the Younger Dryas in the region

(-11,000 to 10,000 BP) (Mayle and Cwynar 1995b).

163 Phase II represents the end of the major isostatic readjustment by the migration of the forebulge through the region. It was during this phase that the stratified Ancestral

Grand Lake was established.

Phase III: -8000 to 3000 BP

At a depth of 19 m below surface the CI/Br ratio decreases to almost the lowest level attained in the GLM-01 core at 5. An AMS date of .7829 ±90 years BP (TO-13068) was obtained from this depth. This date correlates closely with the 8000 BP date

suggested by Kite and Stuckenrath (1986, 1989) for the beginning of the freshwater

Madawaska River draining south over Grand Falls.

At a depth of 16 m dbs an AMS date of 7770 ±80 years BP (TO-13067) was obtained from a wood fragment. From a depth below surface between ~16 and 7 m dbs

grain size increases, indicated by the only representation of gravel above the till. At the

same time LOI decreases to an average of ~1.5%, and the CI/Br ratio could not be

calculated in this portion of the core due to bromide being undetectable, This drop in chloride and bromide, along with a decrease in fines and LOI, can be related to two major

environmental changes within the region. At this time there was an increased contribution of freshwater from the Madawaska River to the north (Kite and Stuckenrath

1986, 1989), as well as a major release of impounded water with the final demise of

Ancestral Grand Lake to the south. If the early impoundment of the lake at ~11,500 BP and its eventual demise at ~ 8000 BP has been interpreted correctly, then a stratified glacial lake existed in the lower Saint John River for ~3500 years.

At approximately 7000 BP there was a lowering of sea-level (base level) (Fader et al. 1977; Shaw et al. 2002) resulting in a significant water level decrease in the Grand

164 Lake basin. The current Bay of Fundy became dry with a lowering of the marine limit from greater than 40 m at the mouth of the Bay to zero at the Bay head (Fader et al.

1977). At this time the Grand Lake Meadows would have been a major freshwater fluvial system, possibly commencing the down-cutting of bedrock at the Reversing Falls and the initial start of the development of today's Grand Lake Meadows.

The Hypsithermal period was between 8500 and 7500 to 4000 and 3300 BP, with a thermal maximum proposed for ~7000 to 6000 BP (Bradstreet and Davis 1975). The

Hypsithermal consisted of a climate that was ~2°C warmer and had a 400 mm decrease in precipitation (Davis et al. 1980), consistent with lower water levels (Sanger et al. 2003).

The beginning of the Hypsithermal is marked in the GLM-01 core by an increase in grain size (gravels) and the percent of LOI decreasing to levels consistent with those found in the till (~1%), both suggesting a period of major climatic fluctuation. In addition, chloride content decreases and bromide is <0.05 mg/L to undetectable, indicating a period of mostly freshwater content, correlating with a marine lowstand (Shaw et al.

2002). The CI/Br ratios were unattainable as any saline water held within the impounded lake had drained to the south. At this time the lower Saint John River valley would only have been influenced by freshwater traveling south, down the Saint John River. By

~3000 BP the percent LOI in the core increases along with a decrease in grain size indicating the end of the dry, arid period of the Hypsithermal.

This early lower Saint John River valley would have consisted of a broad, braided or meandering channel that occupied wide swaths of the available valley. If the river at this time consisted of a braided channel it would have included an intricate network of dividing and rejoining channels separated from one another by sand or gravel bars.

165 Additionally, if the river was more of a meandering river, the result of the unequal distribution of flow velocities across meanders would deposit sand or gravel point bars on the outside of each meander.

This phase consists of a reduction in the CI/Br ratio and LOI with an increase in grain size, all associated with the increased northern contribution of freshwater from the

Madawaska River and final demise of Ancestral Grand Lake. These events lead to the establishment of a more fluvial-dominated system in the Grand Lake Meadows region, likely initiating the beginning of the modern Grand Lake Meadows system and the down- cutting of the Reversing Falls gorge.

Phase IV: -3000 BP to present

From -7 m dbs to surface LOI increases and grain size decreases. LOI continues to steadily increase from a low at the end of the Hypsithermal of ~1% to a high of-6% at

30 cm dbs. Shortly after -5000 BP water levels began to increase, rising rapidly from

-3225 to 2780 BP as a result of more precipitation and lower temperatures (Almquist et al. 2001). As water flow increases, erosion from river and stream banks increases, resulting in a higher sediment load. As the river widens and deepens, fines start to settle out leading to an increase in silts and clays. At -2 m dbs grain size starts to decrease and the CI/Br ratios become measurable indicating marine waters breaching the Reversing

Falls at the mouth of the Saint John River. This would have happened sometime after

3080 ±70 years BP (TO-13064).

The breaching of the Reversing Falls to the south brought with it once more the introduction of saline water to the lower Saint John River and an estuarine environment subject to tidal influences. In addition, the peak in fines may also indicate major

166 freshwater influx, indicative of the end of the Hypsithermal when the precipitation rate increased and there was more freshwater run off overland draining into nearby tributaries and rivers bringing with it a higher sediment load. A substantial amount of freshwater from overland run off and saline water from the breaching of the Reversing Falls would have been carried into the Saint John River at this time leading to the development of the modern estuarine environment.

Chloride and bromide become measurable in the core again at ~7 m dbs allowing for CI/Br ratios to be determined. The CI/Br ratios continue to increase from 2.5 m dbs where ratios were ~25 to 1.5 m dbs where ratios drop off to ~3. This drop in the CI/Br ratio may be representative of a large amount of freshwater from the north traveling through the region at this time from a large flood or floods that may have been two or three times larger than the greatest recorded (Kite and Stuckenrath 1986). At ~ 1 m dbs there is a drop in the CI/Br ratio corresponding with an increase in grain size, indicating faster flowing water. From ~lm dbs to the surface grain size decreases and LOI increases indicative of a modern floodplain.

Phase IV corresponds to the breaching of Reversing Falls allowing saline water to again penetrate into the lower Saint John River valley and Grand Lake basin. This final phase corresponds to the development of the modern lower Saint John River and Grand

Lake Meadows.

167 6.2 Implications of the Geological Interpretations for Archaeological Research

The four phases of deposition within the Grand Lake Meadows since the

Wisconsin deglaciation are in phase with what we know about the major culture history transitions of the lower Saint John River valley (Figure 6.1). The introduction of

Palaeoindian people into the region is linked with the timing of the postglacial DeGeer

Sea (Loring 1980; Dincauze and Jacobson 2001). Analysis of the chloride and bromide from the GLM-01 core suggests that during the Palaeoindian period (prior to 9000 BP) the Grand Lake Meadows region was covered in brackish water. The deposition of fine grained sediment (silt/sandy silt) is also suggestive of deep water over the region.

Palaeoindian sites from Maine, Nova Scotia, Quebec and Ontario have been associated with elevated glacial features such as the strandline of early glacial lakes

(Storck 1984; Bonnichsen et al. 1991), outwash deltas, kame and marine terraces

(MacDonald 1968; Gramly 1982; Spiess and Wilson 1987; Bonnichsen et al. 1991;

Chapdelaine and Bourget 1992). This suggests that areas of site preference were situated at locations where coarse, well-drained sediments were deposited, features that would be elevated and situated well away from the modern lower Saint John River.

Prior to the large regional infrastructure developments that began in the mid- to late 1990s, archaeologically the lower Saint John River valley was one of the most poorly studied parts of the Northeast (Blair 2004, pp. 19-22). Even with the addition of new archaeological information from large-scale consulting archaeology projects and linear corridor surveys, no sites that represent the Palaeoindian culture period are represented in the prehistoric chronological sequence in New Brunswick. Since this region was

168 Phases of deposition Cultural period Radiocarbon date

Figure 6.1: Archaeological cultural history in the context of the stages of deposition within the Grand Lake Meadows with the radiocarbon dates. inundated by deep brackish water during the early part of its history, early site preference in the region may have been on these elevated glacial features. Therefore, the lack of systematic surveys and testing of such features within the lower river valley may be responsible for the absence of evidence for these early post-glacial sites.

Similarly, the Early and Middle Archaic periods (9000 to 5000 BP) are not well- represented in New Brunswick. It has been suggested by Murphy (1998) that Early and

Middle Archaic sites are located in deeply buried contexts, along lakes and rivers with aggrading alluvium. This is similar to what Petersen and Putnam (1992, p. 27) have found in the state of Maine. This may be why no Early or Middle Archaic sites have been identified in some regions; however, the lower Saint John River valley, Grand Lake

Meadows region, was still inundated with deep brackish water at this time. Therefore, early sites in this region would be located well away from the current lakes and rivers.

The importance of marine resources to the Palaeoindian (Tuck 1984; Keenlyside

1985, 1991) and probably to the Early Archaic people (Murphy 1998, p. 83) would have played a role in settlement strategies. Therefore, Early and Middle Archaic site preference for the lower Saint John River valley may have been very similar to site preference for the earlier Palaeoindian people. Additionally, living along the ecological edge of the DeGeer Sea or Ancestral Grand Lake would have allowed for not only terrestrial, but an abundance of marine and freshwater resources. Freshwater fish from rivers and streams flowing into the lake and brackish water fish and/or anadromous fish found within the ancestral lake would have been available to the early inhabitants. Sea mammals as well as other marine resources would also have been available, as Murphy

(1998) notes that seals would have been available to Early and Middle Archaic

170 inhabitants. This suggests that boats would probably have been of great benefit to the early inhabitants of the lower Saint John River valley.

After the demise of Ancestral Grand Lake sometime after -8000 BP the Saint

John River became a freshwater, shallow, fast flowing fluvial system. This was determined from the chloride/bromide and grain size analyses completed from the sediment core. The landscape, and therefore site preference, within the lower Saint John

River valley during this time would have been significantly different than earlier culture periods. Therefore, site preference, possibly as early as the end of the Middle Archaic through the Late Archaic (5000 to 2800 BP), would have been at a much lower elevation, much closer to the banks and floodplain of the modern river system. It is very possible, as Sanger's River Gradient Hypothesis suggests (Sanger 1979), that falls within the lower

Saint John River would have made the river unstable to certain anadromous fish.

Additionally, as noted by the LOI analysis from the GLM-01 core, there was a decrease in organic plant material in the region during this time (the Hypsithermal). This reduction in terrestrial plants, however, may have made reliance on terrestrial animals and water resources more important for those living in the region. There would have been a decline in brackish water resources after the demise of Ancestral Grand Lake; however, there still would have been a large number of freshwater fish available. Today, there are -49 species of freshwater fish known to inhabit inland terrestrial waters

(Carlander 1977). Boats may still have been used by the valley inhabitants along the coast; however, the reliance of boats for people living inland may have declined compared to earlier cultural periods.

171 There were significant palaeogeographic changes in the lower Saint John River valley during the Archaic period as inhabitants would have adapted to a shift from an inland marine environment to a lacustrine environment and finally an inland fluvial environment. Such landscape, environment and resource change would have demanded substantial re-adjustment in settlement and subsistence strategies for local inhabitants altering land use patterns and site selection, as well as activity locations within the lower river valley.

However, sometime after ~ 3000 BP the landscape started to change again with saline water breaching the mouth of the Saint John River at Reversing Falls. The freshwater fluvial system became a tidal-influenced estuarine system. With the rise in sea-level and the development of the modern floodplain, many Late Archaic sites from the lower Saint John River valley may now be underwater or deeply buried with aggrading alluvium. The development of an estuarine environment would have again influenced site preference of precontact people. Therefore, throughout the Maritime

Woodland period (2800 to 500 BP), site preference would have been focused along the modern Saint John River and its floodplain.

6.3 Sea-level Rise

Estuarine studies have been attracting considerable attention in recent years. In addition to their importance from an ecological perspective, increasing attention has been placed on the role these environments play in determining the nature of human - landscape interactions. Landscape studies cover large areas, and thus record phenomena that can answer many of today's global/regional ecological questions. For example,

172 insights about future climatic consequences of the increase in sea-level can be gained from the study of sediment records that occurred during previous times when sea-level fluctuated. On both large and small spatial scales the systems being studied are controlled in large part by long-term temporal processes, recorded in many Quaternary time series.

Isostatic adjustments had a large impact on water level in the lower Saint John

River valley post glaciation. During the Holocene, local isostatic adjustment and global sea-level change has had an effect on water level within the region. A continued rising sea-level could affect coastal aquifers negatively in several ways (Navoy 1991; Nuttle and Portnoy 1992; Ayers et. al 1994; Navoy and Carleton 1995; Oude Essink 1999;

Sherif 1999; Sherif and Singh 1999; Douglas et. al 2001). Perhaps most fundamentally, a landward movement of seawater would push saltwater zones within the coastal aquifers, landward and upward, which could accelerate the rate of saltwater intrusion into aquifers within the lower river valley. In lower elevated areas within the Saint John River valley, sea-level rise may also impact areas of aquifer recharge. Rising sea-levels may cause upstream migration of saltwater within the Saint John River coastal estuary, and additional saline inundation of low-lying areas including the Grand Lake Meadows wetlands and marshes. Sea-level rise may also cause increases in coastal groundwater levels, because of the overall rise in the position of the freshwater-saltwater interface.

This would lead to additional flooding during the spring freshet. Finally, any population increases along the lower Saint John River valley suggest that demands on the ground water resources of the region will grow in the coming years leading to drawdown of existing freshwater aquifers resulting in the incursion of saline water in local wells.

173 A landward movement of seawater as more saline water breaches the Reversing

Falls is not the only concern for the lower Saint John River valley. Additional palaeochannels formed along the coast during periods of lowered sea-level (Flaherty

1989) could also cause a problem. Early coastal rivers eroded underlying sediments as stream channels adjusted to lowered sea-levels. Early palaeochannels are therefore of concern where the rivers breached confining units and the erosional channels then filled with permeable materials as sea-level rose again. In these situations, palaeochannels can provide conduits for the movement of saltwater into freshwater aquifers that underlie the confining units. Palaeochannels have been identified as possible pathways for saltwater intrusion in northern Delaware along the Delaware River (Phillips 1987); the northern

Chesapeake Bay area, Maryland (Chapelle 1985; Drummond 1988; Phillips and Ryan

1989); and the Port Royal Sound area, South Carolina (Landmeyer and Belval 1996;

Foyle et. al. 2001; Krause and Clarke 2001). It is possible that the lower Saint John River may someday be added to this list.

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203 APPENDIX I

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Sample Depth Liquid Plastic Natural Plasticity Liquidity (meter) Limit Limit Water Content (%) Index Index 47.7 30 26 31.26 4 1.3 48.5 30 26 31.47 4 1.4 49.2 32 27 31.81 5 1.0 50 31 27 32.98 4 1.5 50.1 32 27 5 50.4 32 26 50.44 6 4.1 51.2 30 26 34.37 4 2.1 52.4 38 26 40.2 12 1.2 52.7 36 28 39.63 8 1.5 53.8 41 28 38.36 13 0.8 54.3 36 26 38.26 10 1.2 55.3 30 23 31,54 7 1.2 55.8 30 23 30.25 7 1.0 56.9 26 20 34.93 6 2.5 57.3 28 21 27.29 7 0.9 57.8 19 non-plastic 27.88 non-plastic 58.6 20 non-plastic 25.01 non-plastic 59.2 21 APPENDIX IV

X-RAY DIFFRACTION RESULTS X-Ray Diffraction Results

Sample Depth Laboratory Mineral (meter) Sample Number Composition 19.2024 31-756 Quartz, Muscovite, Albite, Clinochlore 19.685 32-775 Quartz, Muscovite, Albite, Clinochlore 20.2438 . 33-797 Quartz, Muscovite, Albite, Clinochlore, Calcite 21.0312 35-828 Quartz, Muscovite, Albite, Clinochlore 21.4884 36-846 Quartz, Muscovite, Albite, Clinochlore 22.0726 37-869 Quartz, Muscovite, Albite, Clinochlore 22.7076 38-894 Quartz, Muscovite, Albite, Clinochlore, Orthoclase 23.5204 39-926 Quartz, Muscovite, Albite, Clinochlore, Orthoclase 24.13 40-950 Quartz, Muscovite, Albite, Clinochlore 24.6888 41-972 Quartz, Muscovite, Albite, Clinochlore 25.527 42-1006 Quartz, Muscovite, Albite, Clinochlore, Calcite 26.4668 44-1042 Quartz, Muscovite, Albite, Clinochlore 27.1272 45-1068 Quartz, Muscovite, Albite, Clinochlore, Calcite, Orthoclase 27.7368 46-1092 Quartz, Muscovite, Albite, Clinochlore, Calcite, Orthoclase 28.194 47-1140 Quartz, Muscovite, Albite, Clinochlore, Calcite 28.956 48-1140 Quartz, Muscovite, Albite, Clinochlore 29.5656 49-1164 Quartz, Muscovite, Albite, Clinochlore 31.5468 53-1242 Quartz, Muscovite, Albite, Clinochlore, Calcite 32.3088 54-1272 Quartz, Muscovite, Albite, Clinochlore, Calcite 33.0708 55-1302 Quartz, Muscovite, Albite, Clinochlore 33.8328 56-1332 Quartz, Muscovite, Albite, Clinochlore 34.5948 57-1362 Quartz, Muscovite, Albite, Clinochlore, Calcite 35.5092 58-1398 Quartz, Muscovite, Albite, Clinochlore, Calcite 37.4904 61-1476 Quartz, Muscovite, Albite, Clinochlore, Orthoclase 38.4048 62-1512 Quartz, Muscovite, Albite, Clinochlore, Orthoclase 39.0144 63-1536 Quartz, Muscovite, Albite, Clinochlore, Calcite, Orthoclase 40.5384 65-1596 Quartz, Muscovite, Albite, Clinochlore, Calcite 41.4528 66-136 Vivianite 41.4528 66-1632 Quartz, Muscovite, Albite, Clinochlore 42.0878 67-1657 Quartz, Muscovite, Albite, Clinochlore, Calcite 43.0276 68-1694 Quartz, Muscovite, Albite, Clinochlore, Calcite, Orthoclase 43.7388 69-1722 Quartz, Muscovite, Albite, Clinochlore, Orthoclase 44.5516 70-1754 Quartz, Muscovite, Albite, Clinochlore, Calcite 45.2628 71-1782 Quartz, Muscovite, Albite, Clinochlore, Calcite 45.8978 72-1807 Quartz, Muscovite, Albite, Clinochlore, Calcite, Orthoclase 46.7868 74-1842 Quartz, Muscovite, Albite, Clinochlore, Calcite 47.5996 75-1874 Quartz, Muscovite, Albite, Clinochlore, Calcite 48.3108 76-1902 Quartz, Muscovite, Albite, Clinochlore, Calcite 49.0728 77-1932 Quartz, Muscovite, Albite, Clinochlore, Calcite 49.8348 78-1962 Quartz, Muscovite, Albite, Clinochlore, Orthoclase 50.5968 79-1992 Quartz, Muscovite, Albite, Clinochlore, Orthoclase 51.3588 80-2022 Quartz, Muscovite, Albite, Clinochlore, Orthoclase 52.1208 81-2052 Quartz, Muscovite, Albite, Clinochlore 52.9336 82-2084 Quartz, Muscovite, Albite, Clinochlore, Orthoclase 53.6448 83-2112 Quartz, Muscovite, Albite, Clinochlore 54.4068 84-2142 Quartz, Muscovite, Albite, Clinochlore 55.0418 85-2167 Quartz, Muscovite, Albite, Clinochlore 55.88 86-2200 Quartz, Muscovite, Albite, Clinochlore, Calcite 56.5658 87-2227 Quartz, Muscovite, Albite, Clinochlore, Calcite, Orthoclase 57.4548 88-2262 Quartz, Muscovite, Albite, Clinochlore, Orthoclase 58.2168 89-2292 Quartz, Muscovite, Albite, Clinochlore, Orthoclase 58.8518 90-2317 Quartz, Muscovite, Albite, Clinochlore, Calcite, Orthoclase Sample 31-756"

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2-Theta - Scale BSsample 31-756" - File: Pam_31-756.RAW - Type: 2Th/Th locked - Start: 5.000 • - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta 5.000 • - Theta 2.500 • Operations: Background 1.000,1.0001 Import DHI46-1045 (')- Quartz, syn - Si02 - Y: 100.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-P3221 (154)-3-113.01 [jj]07-0042 (I) - Muscovite-3T - (K,Na)(AI,Mg,Fe)2(Si3.1 AI0.9)O10(OH)2 - Y: 12.50 % - d x by: 1. - WL: 1.5406 - Hexagonal - a 5.203 - b 5.20300 - c 29.986 - alpha 90.000 - beta 90.000 - gamma 120.000 - Pri Qj]09-O466n-Albite, ordered - NaAISi308 - Y: 22.92 %-dxby:1.- WL: 1.5406-Triclinic-a8.144-b 12.787- C7.160 -alpha94.26-beta 116.6-gamma87.67-Base-centred-C-1 (0)-4-664.837-l/lc [B29-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 12.50 % - d x by: 1. - WL: 1.5406 - Monoclinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 -gamma 90.000 - Base-centred - Sample 32-775"

03 C 3 500 O O LI u. 2-Theta - Scale fflsample 32-775" - File: Pam_32-775.RAW - Type: 2Th/Th locked - Start: 5.000 • - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 "C (Room) - Time Started: 0 s - 2-Theta 5.000 • - Theta 2.500 • Operations: Background 1.000,1.0001 Import [U46-1045 (')- Quartz, syn - Si02 - Y: 97.92 %- d x by: 1. - WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-P3221 (154)-3-113.010 H307-0042 (I) - Muscovite-3T - (K,Na)(AI,Mg,Fe)2(Si3.1AI0.9)O10(OH)2 - Y: 10.42 % - d x by: 1. - WL: 1.5406 - Hexagonal - a 5.203 - b 5.20300 - C29.988 - alpha 90.000- beta 90.000 -gamma 120.000 - Pri Qj] 09-0466 (*) - Albite, ordered - NaAISi308 - Y: 11.72 %- d x by: 1. - WL: 1.5406 - Tridinic - a 8.144 - b 12.787 - c 7.160 - alpha 94.26 - beta 116.6 - gamma 87.67-Base-centred - C-1 (0)-4-664.837-l/lc [029-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 8.33 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Base-centred - Sample 33-797"

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2-Theta - Scale KlSample 33-797' - File: Pam_33-797.RAW - Type: 2Th/Th locked - Start: 5.000 • - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 "C (Room) - Time Started: 10 s- 2-Theta 5.000 • - Theta 2.500 Operations: Background 1.000,1.0001 Import 0346-1045 (') -Quartz. syn-Si02-Y:100.00 %-dxby: 1.-WL: 1.5406- Hexagonal -a4.91344-b4.91344-c5.40524 -alpha 90.000-beta 90.000-gamma 120.000 - Primitive-P3221 (154) -3 -113.01 [Q06-0263(l)-Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2-Y:4.51 %-dxby: 1.-WI: 1.5406 - Monoclinic - a 5.19-b 9.03-c 20.05-alpha 90.000-beta 95.77-gamma 90.000-Base-centred-C2/C (15)-4 Hj)09-0466C)-Albite, ordered - NaAISi308- Y: 8.33% -dxby: 1.-WL: 1.5406-Tridinic-a8.144-b12.787-c7.160- alpha94.26-beta 116.6-gamma87.67- Basa«intred - C-1 (0)-4-664.837-l/IcP [B29-O701 (I) - Clinochlore-1 Mllb. ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 5.21 % - d x by: 1. - WL: 1.5406 - Monoclinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Base-centred - i) '147-1743 (C) - Calcite - CaC03 - Y: 2.08 %- d x by: 1.- WL: 1.5406 - Hexagonal (Rh) - a 4.9896 - b 4.98960 - c 17.0610 - alpha 90.000 - beta 90.000 - gamma 120.000-Primibve-R-3c (167)-6-367.846 Sample 35-825

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2-Theta - Scale BSsample 35-825 - File: Pam_35-828.RAW - Type: 2Th/Th locked - Start: 5.000 • - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 "C (Room) - Time Started: 0 s - 2-Theta: 5.000 • - Theta: 2.500 • Operations: Background 1.000,1.0001 Import [0)46-1045 (*)- Quartz, syn - Si02 - Y: 50.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.00O-Primitive-P3221 (154)-3-113.010 [D06-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 4.17 % - d x by: 1. - WL: 1.5406 - Monoclinic - a 5.19 - b 9.03 -c 20.05 - alpha 90.000 - beta 95.77 - gamma90.000 - Base-centred - C2/C (15) -4 CLD 09-0466 (*)- Albite, ordered -NaAISi308-Y: 14.58 %-dxby: 1.- WL 1.5406 -Triclinic-a8.144- b 12.787 -c 7.160 -alpha 94.26 -beta 116.6 -gamma 87.67-Base-centred - C-1 (0)-4-664.837-l/lc Q]]29-O701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si.AI)4O10(OH)8 - Y: 6.25 % - d xby: 1. - WL: 1.5406 - Monoclinic- a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma90.000 - Base-centred - Sample 36-846

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2-Theta - Scale BSsample 36-846 - File: Pam_36-846.RAW - Type: 2Th/Th locked • Start 5.000 • - End: 70.000 • - Step: 0.020 * - Step time: 0.5 s - Temp.: 25 "C (Room) - Time Started: 0 s - 2-Theta: 5.000 • - Theta: 2.500 • Operations: Background 1.000,1.0001 Import Q]l46-1045 (') -Quartz, syn-Si02-Y: 100.00 %-dxby: 1.-WL: 1.5406 -Hexagonal -a 4.91344 -b 4.91344 -C5.40524- alpha 90.000- beta 90.000-gamma 120.000- Primitive -P3221 (154) -3 -113.01 Hi|06-0263(l)-Muscovite-2M1 - KAI2(Si3AI)O10(OH.F)2-Y: 4.69 % -d xby: 1. -WL: 1.5406-Monodinic-a5.19-b9.03-c20.05 -alpha 90.000-beta95.77-gamma90.000-8ase-centred-C2/o(15)-4 Hil09-0466 (*) - Albite, ordered - NaAISi308 - Y: 12.50 %-dxby: 1.-WL 1.5406 -Triclinic-a8.144-b12.787-c7.160-alpha 94.26 -beta 116.6-gamma 87.67- Base-centred - C-1 (0)-4-664.837-l/lc H329-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 8.33 % - d x by: 1. - WL: 1.5406 - Monoclinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Base-centred - Sample 37-869

2-Theta - Scale ffilsample 37-869 - File: Pam_37-869.RAW - Type: 2Th/Th locked - Start 5.000 • - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 'C (Room) - Time Started: 0 s - 2-Theta 5.000 • - Theta: 2.500 • Operations: Background 1.000,1.0001 Import [046-1045 (•). Quartz, syn - Si02 - Y: 100.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-P3221 (154)-3-113.01 [0 06-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 6.25 %- d xby: 1. - WL: 1.5406 - Monoclinic - a 5.19 - b 9.03 -c 20.05 - alpha 90.000-beta95.77-gamma90.000-Base-centred-C2/c(15)-4 Qj]09-0466O-Albite, ordered- NaAISi308-Y: 12.50 %-dxby: 1.-WL: 1.5406-Triclinic-a8.144-b 12.787-c7.160 -alpha 94.26 -beta 116.6-gamma 87.67- Base-centred - C-1 (0)-4-664.837-He [029-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 6.25 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Base-centred - Sample 38-894

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2-Theta - Scale fflsample 38-894 - File: Pam_38-894.RAW - Type: 2Th/Th locked - Start 5.000 • - End: 70.000 • - Step: 0.020" - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta 5.000 * - Theta: 2.500 • Operations: Background 1.000,1.000| Import 0346-1045 (•) - Quartz, syn - Si02 - Y: 100.00 % - d x by: 1. - WL: 1.5406 - Hexagonal -a4.91344-b4.91344-c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P3221 (154) - 3 -113.01 Qj]06-0263(l)-Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2-Y: 6.25% -dxby: 1.-WL: 1.5406-Monoclinic-a5.19-b9.03-c20.05 -alpha 90.0M-beta95.77-gamma90.00O-Base-cantred-C2/c(15)-4 Hil09-04S6 (*) - Albite. ordered - NaAISi308 - Y: 18.75 %-dxby: 1.-WL 1.5406-Tridinio-a8.144-b12.787-c7.160 -alpha 94.26 -beta 116.6 -gamma 87.67- Base-centred - C-1 (0)-4-664.837-l/lc DJ)29-0701 (I) - dinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 12.50 % - d x by: 1. - Wl_: 1.5406 - Monoclinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Base-centred - llil 19-0002 (I) - Orthoclase, ban an - (K,Ba,Na)(Si,AI)408 - Y: 8.33 %- d x by: 1. - WL: 1.5406 - Monoclinic - a 8.552 - b 13.040 - c 7.200 - alpha 90.000-beta 115.7-gamma 90.000-Base-centred-C2/m (12) Sample 39-926

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2-Theta - Scale KlSample 39-926 - File: Pam_39-926.RAW - Type: 2Th/Th locked - Start 5.000 • - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 "C (Room) - Time Started: 0 s - 2-Theta: 5.000 ° - Theta 2.500 • Operations: Background 1.000,1.0001 Import HD46-1045 (') - Quartz, syn - Si02 - Y: 100.00 %- d x by: 1.- WL: 1.5408 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-P3221 (154)-3-113.01 006-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 6.25 % - d x by: 1. - WL: 1.5406 - Monoclinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000 - beta 95.77 - gamma 90.000 - Base-centred - C2/C (15) - 4 DID 09-0466 (*)- Albite, ordered - NaAISi308 - Y: 18.75 %- d x by: 1.- WL: 1.5406 - Triclinic - a 8.144 - b 12.787 - c 7.160 - alpha 94.26 - beta 116.6 - gamma 87.67-Base-centred - C-1 (0)-4-664.837-l/lc 0329-0701 (l)-Clinochlore-1Mllb.ferroan-(Mg,Fe)6(Si,AI)4O10(OH)8-Y:10.42%-dxby:1.-WL: 1.5406-Monodinic-a5.36-b9.28-c14.2-alpha90.000-beta97.15-gamma 90.000- Base-centred - llil 19-0002 (I) - Orthoclase, barian - (K,Ba,Na)(Si,AI)408 - Y: 4.17 % - d x by: 1. - WL: 1.5406 - Monoclinic - a 8.552 - b 13.040 - c 7.200 - alpha 90.000 - beta 115.7 - gamma 90.000 - Base-centred - C2/m (12) Sample 40-950

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2-Theta - Scale fflsample 40-950 - File: Pam_40-950.RAW - Type: 2Th/Th locked - Start: 5.000 • - End: 70.000 • - Step: 0.020 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta 5.000 • - Theta: 2.500 • Operations: Background 1.000,1.0001 Import [046-1045 (*) - Quartz, syn - Si02 - Y: 97.92 % - d x by: 1. - WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P3221 (154) - 3 -113.010 GJ]06-O263 (I) - Muscowte-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 12.50 % - d xby: 1. - WL: 1.5406 - Monodinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000 - beta 95.77 - gamma 90.000 - Base-centred - C2/C (15) - [Ho9-0466(*)-Albite, ordered - NaAISi308- Y: 20.83 %-dxby:1.- WL: 1.5406-Tridinic-a8.144-b 12.787-c7.160-alpha94.26 -beta 116.6 -gamma87.67-Base-centred-C-1 (0)-4-664.837-l/Ic [029-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 16.67 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 -gamma 90.000 - Base-centred - Sample 41-972

to "£ 800 o O 700

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2-Theta - Scale ElSample 41-972 - File: Pam_41-972.RAW - Type: 2Th/Th locked - Start: 5.000 • - End: 70.000" - Step: 0.020 * - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta 5.000 • - Theta 2.500 • Operations: Background 1.000,1.0001 Import D346-1045 (•)- Quartz, syn - Si02 - Y: 95.83 %- d x by: 1. - WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha90.000 -beta 90.000 -gamma 120.000 - Primitive-P3221 (154)-3-113.010 H0O6-O263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 8.33 % - d x by: 1. - WL: 1.5406 - Monoclinic - a 5.19 - b 9.03 -c 20.05 - alpha 90.000 - beta 95.77 - gamma90.000 - Base-centred - C2/c (15) -4 QZD 09-0466 (•) - Albite, ordered - NaAISi308 - Y: 25.00 %- d x by: 1. - WL: 1.5406 - Tridinic - a 8.144 - b 12.787 - c 7.160 - alpha 94.26 - beta 116.6 - gamma 8737-Base-centred-C-1 (0)-4-664.837-l/lc H329-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si.AI)4O10(OH)8 - Y: 12.50 % - d x by: 1. - WL: 1.5406 - Monoclinic - a 5.36 - b 9.28 -c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Base-centred - Sample 42-1006

2-Theta - Scale ffl Sample 42-1006 - File: Pam_42-1006. RAW - Type: 2Th/Th locked - Start: 5.000 • - End: 70.000' - Step: 0.020" - Step time: 0.5 s - Temp.: 25 "C (Room) - Time Started: 0 s - 2-Theta 5.000 • - Theta: 2.50 Operations: Background 1.000,1.0001 Import 046-1045 (')- Quartz, syn - Si02 - Y: 93.75 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524. alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-P3221 (154)-3-113.010 03 06-0263 (I) - Muscovite-2M 1 - KAI2(Si3AJ)010(OH,F)2 - Y: 8.33 %- d x by: 1.- WL: 1.5406 - Monoclinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000-beta 95.77-gamma 90.000-Base-centred-C2/C (15)-4 [Lil09-0466n-Albite, ordered-NaAISi308-Y: 16.67 %-dxby: 1.-WL: 1.5406-Triclinic-a8.144-b12.787-c7.160 -alpha 94.26 -beta 116.6-gamma 87.67-Base-centred-C-1 (0) -4 -664.837 -l/lc [029-0701 (I) -Clincchlore-1Mllb,ferroan-(Mg,Fe)6(Si,AI)4O10(OH)8-Y: 10.42 %-dxby: 1.-WL: 1.5406 -Monoclinic-a 5.36-b 9.28 -c 14.2 -alpha 90.000 - beta 97.15-gamma 90.000-Base

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2-Theta - Scale fflsample 44-1042 - File: Pam_44-1042. RAW - Type: 2Th/Th locked - Start: 5.000" - End: 70.000 • - Step: 0.020" - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta 5.000 • - Theta 2.50 Operations: Background 1.000,1.0001 Import 046-1045 (*)-Quartz, syn-Si02-Y: 100.00 % -d xby: 1.-WL: 1.5406-Hexagonal-a4.91344-b4.91344-c5.40524-alpha90.000-beta90.000-gamma 120.000-Primitive-P3221 (154)-3-113.01 DJ]06-0263 (I) - Muscovite-2M1 -KAI2(Si3At)O10(OH,F)2-Y: 5.21 %-d xby: 1.-WL: 1.5406- Monoclinic-a 5.19-b 9.03-c 20.05-alpha 90.000-beta 95.77-gamma 90.000- Base-centred-C2/C (15) -4 Hil09-0466 (*)- Albite, ordered - NaAISi308 - Y: 20.83 %- d x by: 1.- WL: 1.5406 - Triciinic - a 8.144 - b 12.787 - c 7.160 -alpha 94.26 - beta 116.6 - gamma 87.67-Base-centred - C-1 (0)-4-664.837-Iflc Qj]29-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 8.33 % - d x by: 1. - WL: 1.5406 - Monoclinic- a 5.36 - b 9.28 - c 14.2 - alpha 90.000- beta 97.15 - gamma 90.000 - Base-centred - Sample 45-1068

2-Theta - Scale BSsample 45-1068 - File: Pam_45-1068.RAW - Type: 2Th/Th locked - Start: 5.000 * - End: 70.000' - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 *C (Room) - Time Started: 0 s - 2-Theta: 5.000 • - Theta 2.50 Operations: Background 1.000,1.0001 Import •346-1045 (*)- Quartz, syn - Si02 - Y; 100.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000-gamma 120.000-Primitive-P3221 (154)-3-113.01 D306-0263 (I) - Muscowte-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 10.42 %-d x by: 1. - WL: 1.5406 - Monodinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000 - LHIo9-0466(*)-Alblte, ordered -NaAISi 308- Y: 16.67 %-dxby: 1.-WL: 1.5406-Tridinic-a8.144-b12787-c7.160 -alpha 94.26-beta 116.6-garmiia 87.67-Base-centred - C-1 (0)-4-664.837-l/lc [Q29-0701 (I) - Clincchlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 14.58 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Base-centred - L01l 9-0002 (I) - Orthoclase, bari an - (K,Ba,Na)(Si,AI)408 - Y: 8.50 %- d x by: 1.- WL: 1.5406 - Monodinic - a 8.552 - b 13.040 - c 7.200 - alpha 90.000-beta115.7-gamma90.000-Base-centred-C2/m(12) (EH 05-0586 (•)- Caldte, syn - CaC03 - Y: 4.17 %- d x by: 1.- WL: 1.5406 - Hexagonal (Rh) - a 4.989 - b 4.98900 - c 17.062 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-R-3c (167)-6-367.78 Sample 46-1092

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2-Theta - Scale BSsample 46-1092 - File: Pam_46-1092.RAW - Type: 2WTh locked - Start: 5.000 • - End: 70.000" - Step: 0.020 * - Step time: 0.5 s - Temp.: 25 "C (Room) - Time Started: 0 s - 2-Theta 5.000 • - Theta 2.50 Operations: Background 1.000,1.0001 Import [046-1045 (*)- Quartz, syn - Si02 - Y: 100.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - o 5.40524 - alpha 90.000 - beta 90.000-gamma 120.000-Primiiive-P3221 (154)-3-113.01 D3 06-0263 (I) - Muscovite-2M1 - KAJ2(Si3AI)O10(OH,F)2 - Y: 8.33 %- d x by: 1. - WL: 1.5406 - Monoclinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000 - beta 95.77-gamma 90.000-Base-centred-C2/C (15)-4 Dal 09-0466 (') -Albite, ordered-NaAISi308-Y: 18.75 %-dxby: 1.-WL 1.5406-Triclinic-a8.144-b12.787-c7.160-alpha 94.26 -beta 116.6-gamma87.67-Base-centred - C-1 (0)-4-664.837-l/lc 029-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 12.50 % - d x by: 1. - WL: 1.5406 - Monoclinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Base-centred - Dal 19-0002 (I) - Orthoclase, barian - (K,Ba,Na)(Si,AI)408 - Y: 6.25 %- d x by: 1.- WL: 1.5406 - Monoclinic - a 8.552 - b 13.040 - c 7.200-alpha90.000-beta115.7-gamma90.000-Base

.—-. 900 g 8°°

~X 700

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2-Theta - Scale ffilSample 47-1140 - File: Pam_47-1110.RAW - Type: 2Th/Th locked - Start 5.000 ° - End: 70.000 • - Step: 0.020 • - Step time 0.5 s - Temp.: 25 "C (Room) - Time Started: 0 s - 2-Theta 5.000 ° - Theta 2.50 Operations: Background 1.000,1.0001 Import 046-1045 (')- Quartz, syn - Si02 - Y: 100.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000-gamma 120.000-Primitive-P3221 (154)-3-113.01 Qjl 06-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 4.17 % - d xby: 1. - WL: 1.5406 - Monoclinic- a 5.19 - b 9.03 - c 20.05 - alpha 90.000-beta 95.77-gamma 90.000-Base-centred-C2/c (15)-4 IB 09-0466 (')- Albite, ordered - NaAISi308 - Y: 35.42 %- d x by: 1.- WL 1.5406 - Tridinic - a 8.144 - b 12.787 - c 7.160 - alpha 94.26 - beta 116.6 - gamma 87.67-Base-centred - C-1 (0)-4-664.837-l/lc [029-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 6.25 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Bas¢red - llli05-0586 (*)- Calcite, syn - CaC03 - Y: 4.17 %- d x by: 1.- WL: 1.5406 - Hexagonal (Rh) - a 4.989 - b 4.98900 - c 17.062 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-R-3c (167)-6-367.78 Sample 48-1140 I

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2-Theta - Scale ESsample 48-1140 - File: Pam_48-1140.RAW - Type: 2TWTh locked - Start 5.000 ° - End: 70.000 ° - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 X (Room) - Time Started: 0 s - 2-Theta 5.000 • - Theta 2.50 Operations: Background 1.000,1.0001 Import 0346-1045 (') - Quartz, syn - Si02 - Y: 100.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 -gamma 120.000-Primitive-P3221 (154)-3-113.01 Q3 06-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 10.42 %- d x by: 1. - WL: 1.5406 - Monodinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000-beta 95.77-gamma 90.000-Base<»itred-C2/c (15)- 03 09-0466 (')-Albite, ordered -NaAISi 308- Y: 10.42 %-dxby: 1.-WL: 1.5406-Tridinic-a8.144-b12.787-c7.160-alpha94.26-beta116.6-garrima87.67-Base

2-Theta - Scale Elsample 49-1164 - File: Pam_49-1164.RAW - Type: ZTWTh locked - Start 5.000 * - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 "C (Room) - Time Started: 0 s - 2-Theta 5.000 • - Theta 2.50 Operations: Background 1.000,1.0001 Import 0346-1045 (')- Quartz, syn - Si02 - Y: 100.00 %- d xby: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344- c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive-P3221 (154)-3-113.01 [Q0&O263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 6.25 % - d x by: 1. - WL: 1.5406. Monoclinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000 - beta 95.77 - gamma 90.000 - Bas¢red - C2/C (15) - 4 Qjj 09-0466 (•)- Albite, ordered - NaAISi 308 - Y: 12.50 %- d x by: 1. - WL: 1.5406 - Tridinic - a 8.144 - b 12.787 - c 7.160 - alpha 94.26 - beta 116.6 - gamma 87.67-Base^entred-C-1 (0)-4-664.837-Wc LH129-0701 (l)-aincchlore-1Mllb,ferroan-(Mg,Fe)6(Si,AI)4O10(OH)8-Y: 12.50%-dxby: 1.-WL: 1.5406-Moncidinic-a5.36-b9.28-c14.2-alpha90.000-beta97.15-gamrna90.000-Bas¢red- Sample 53-1242

5 10 20 30 40 50 60 7C 2-Theta - Scale BSsample 53-1242 - File: Pam_53-1242.RAW - Type: 2Th/Th locked - Start 5.000" - End: 70.000 ° - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta 5.000 • - Theta 2.50 Operations: Background 1.000,1.0001 Import [0146-1045 (')- Quartz, syn - Si02 - Y: 100.00 % -d x by: 1. -WL: 1.5406- Hexagonal -a4.91344 -b 4.91344 -c 5.40524 -alpha 90.000- beta 90.000-gamma 120.000-Primitive-P3221 (154)-3-113.01 [Q10-0393 (•)- Albite, disordered - Na(Si3AI)08 - Y: 14.06 %- d x by: 1.- WL: 1.5406 - Triclinic - a 8.165 - b 12.872 - c 7.111 - alpha 93.45 - beta 116.4-gamma 90.28 - Bas¢red-C-1 (0)-4-667.792- Qj) 06-0263 (I) - Muscovite-2M1 -KAI2(Si3AI)O10(OH,F)2-Y: 16.67 %-dxby: 1.-WL: 1.5406- Mmodinic-a5.19-b9.03-c20.05-alpha90.000-bea95.77-gaiinma 90.000-Base-centred-C2/c(15)- 0329-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 18.75 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Base-centred - III] 05-0586 (*) - Calcite, syn - CaC03 - Y: 7.81 % - d x by: 1. - WL: 1.5406 - Hexagonal (Rh) - a 4.989 - b 4.98900 - c 17.062 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - R-3c (167) - 6 - 367.78 Sample 54-1272

to c D 700 o r- 600

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2-Theta - Scale fflSample 54-1272 - File: Pam_54-1272.RAW - Type: 2Th/Th locked - Start 5.000 ° - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta 5.000' - Theta 2 Operations: Background 1.000,1.0001 Import [046-1045 (')- Quartz, syn - Si02 - Y: 97.92 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000-gamma 120.000-Primitive-P3221 (154)-3-113 HD 09-0466 (*)- Albite, ordered - NaAISi308 - Y: 25.00 %- d x by: 1.- WL: 1.5406 - Triclinic - a 8.144 - b 12.787 - c 7.160 - alpha 94.26 - beta 116.6 - gamma 67.67 - Base

600 -

500 -

ST 400 - c Zl O oc - _1 300 -

200 -

100 —

0 J j> J r l j I i i tp^iyji

2-Theta - Scale ffijsample 55-1302 - File: Pam_55-1302.RAW - Type: 2Th/Th locked - Start: 5.000 • - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 *C (Room) - Time Started: 0 s - 2-Theta 5.000 • - Theta 2 Operations: Background 1.000,1.0001 Import Q]]'l6-1045(*)-Quart2,syn-SiO2-Y:100.00%-dxby:1.-WL: 1.5406-Hexagonal-a4.91344-b4.91344-o5.40524-alpha90.000-oeta90.000-gamma 120.000- Primitive-P3221 (154)-3-11 Qj]09-O466 (•) - Albite, ordered - NaAISi308 - Y: 16.67 % - d x by: 1. - WL: 1.5406 - Tridinic - a 8.144 - b 12.787 - c 7.160 - alpha 94.26 - beta 116.6 - gamma 87.67 - Basfrcentred - C-1 (0) - 4 - 664.837 - Qj] 06-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 -Y: 12.50 %- d x by: 1. -WL: 1.5406 - Monoclinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000-beta 95.77-gamma 90.000-Base-centred-C2/c(1 Q]]29-0701 (I) - ainochlore-1Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 14.58 % - d x by: 1. - WL: 1.5406 - Monoclinic -a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Sample 56-1332

2-Theta - Scale ElSample 56-1332 - File: Pam_56-1332.RAW - Type: 2Th/Th locked - Start: 5.000 ° - End: 70.000 • - Step: 0.020 * - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta: 5.000 ° - Theta: 2 Operations: Background 1.000,1.0001 Import Qj]46-1045C)-Qjartz, syn-Si02-Y: 100.00%-dxby: 1.-WL: 1.M06-Hexagmal-a4.91344-b4.91344-c5.40524-alpra90.000-beta90.000-gamma 120.000-Prirritive-P3221 (154)-3-11 HO 09-0466 (')- Albite. ordered - NaAISi308 - Y: 11.28 %- d x by: 1. - WL: 1.5406 - Triclinic - a 8.144 - b 12.787 - c 7.160 - alpha 94.26 - beta 116.6 - gamma87.67 - Base-centred - C-1 (0)-4-664.837- IE29-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 6.25 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Base-centre H306-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 8.33 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000 - beta 95.77 - gamma 90.000 - Base-centred - C2/C (15 Sample 57-1362

2-Theta - Scale Bsample 57-1362 - File: Pam_57-1362.RAW - Type: 2Th/Th locked - Start 5.000 • - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 "C (Room) - Time Started: 0 s - 2-Theta 5.000 * - The Operations: Background 1.000,1.0001 Import HB46-1045 (*)- Quartz, syn - Si02 - Y: 93.75 %- d x by: 1.- WL 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000-gamma 120.000 - Primitive-P3221 (154)-3- 009-0466 (*)-«bite, ordered-NaAISi308-Y: 12.50%-dxby: 1.-WL: 1.5406-Tridinic-a8.144-b12.787-c7.160-alpha94.26-beta116.6-g^rrima87.67.Base-oantred-C-1 (0)-4-664.8 [Q 06-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH.F)2 - Y: 5.16 % - d x by: 1. - WL: 1.5406 - Monoclinic - a 5.19 - b 9.03-c 20.05-alpha 90.000-beta 95.77-gamma 90.000-Base-centred-C2/C [Q 29-0701 (I) - Clincchlore-1 Mllb, ferroan - (Mg, Fe)6(Si,/>J)4010(OH)8 - Y: 14.58 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.36 - b 9.28-c 14.2-alpha 90.000-beta 97.15-gamma 90.000-Base- [0 05-0586 (*)- Calcite, syn - CaC03 - Y: 2.59 %- d x by: 1.- WL: 1.5406 - Hexagonal (Rh) - a 4.989 - b 4.98900 - c 17.062 - alpha 90.000 - beta 90.000-gamma 120.000-Primitive-R-3c (167)-6- Sample 58-1398

5 10 20 30 40 50 60 7( 2-Theta - Scale BBsample 58-1398 - File: Pam_58-1398.RAW - Type: 2Th/Th locked - Start 5.000 ° - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta: 5.000" - The Operations: Background 1.000,1.0001 Import [046-1045 (*)-Quani, syn - Si02 - Y: 89.58 %-d x by: 1.-WL: 1.540* - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120^ EH 09-0466 (')- Albite, ordered - NaAISi308 - Y: 12.74 %- d x by: 1. - WL: 1.5406 - Triclinic - a 8.144 - b 12.787 - c 7.160 - alpha 94.26 - beta 116.6 - gamma 87.67-Base-centred-C-1 (0)-4-664.8 [Q06-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 9.37 % - d x by: 1. - WL: 1.5406 - Monoclinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000 - beta 95.77 - gamma 90.000 - Base-centred. C2/c [029-0701 (l)-Clina*lore-1Mllb,ferroan-(Mg,Fe)6(Si,AIH^^ !Lllo5-0586 (*) - Calcite, syn - CaC03 - Y: 1.69 % - d x by; 1. - WL: 1.5406 - Hexagonal (Rh) - a 4.989 - b 4.98900 - c 17.062 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - R-3C (167) - 6 - Sample 61-1476

2-Theta - Scale fflSampIS 61-1476 - File: Pam_61-1476.RAW- Type: 2Th/Th locked - Start: 5.000 • - End: 70.000 • - Step: 0.020 ° - Step time: 0.5 s - Temp.: 25 °C (Room) -Time Started: 0 s - 2-Theta: 5.000 * - Theta 2.50 Operations: Background 1.000,1.0001 Import 0346-1045 (')- Quartz, syn - Si02 - Y: 95.83 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-P3221 (154)-3-113.010 HD06-0263(I)-Muscovite-2M1 -K«2(Si3AI)O10(OH,F)2-Y: 27.08%-dxby: 1.-WL: 1.5406.Monodinic-a5.19-b9.03-c20.05-alpha90.000-beta95.77-gamma90.000-Base-centred-C2/c(15)- Qj] 09-0466 (')-Albite, ordered -NaAISi 308- Y: 16.67 %-dxby: 1.-WL: 1.5406-Triclinic-a8.144-b12.787-c7.160 -alpha 94.26-beta 116.6-gamma 87.67-Base-centred - C-1 (0)-4-664.837-Iflc D329-0701 (I) - dinochlore-1 Mllb. ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 35.42 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Base-centred - LLH 19-0002 (I) - Orthodase. barian - (K, Ba,Na)(Si,AI)408 - Y: 4.17 % - d x by: 1. - WL: 1.5406 - Monodinic - a 8.552 - b 13.040 - c 7.200-alpha90.000-beta115.7-gamma 90.000-Base-cenlred-C2/m(12) Sample 62-1512

800 "3

700 -j

600 "3

500 -H

400 "3

300 -3

200 "3

100 "3

0 5 10 20 30 40 50 60 7C 2-Theta - Scale fflsample 62-1512 - File: Pam_62-1512.RAW - Type: 2Th/Th locked - Start 5.000 • - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta: 5.000 • - Theta 2.50 Operations: Background 1.000,1.0001 Import 046-1045 (*)- Quartz, syn - Si02 - Y: 100.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a4.91344 - b 4.91344 - c 5.40524 - alpha 90.000-beta 90.000-gamma120.000-Primitjve-P3221 (154)-3-113.01 Qj|u6-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 14.58 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.19 - b 9.03 - C20.05 - alpha 90.000 - beta 95.77 - gamma 90.000 - Base-centred - C2/C (15) - EH 09-0466 (*)- Albite, ordered - NaAISi308 - Y: 22.92 %- d xby: 1. - WL: 1.5406 -Triclinic - a8.144 - b 12.787 - c 7.160 -alpha 94.26 - beta 116.6 -gamma 87.67-Base-centred - C-1 (0)-4-664.837-l/lc 029-0701 (I) - Qinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 22.92 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Base-centred - lllli 19-0002 (I) - Orthoclase, barian - (K.Ba,Na)(Si,AI)408 - Y: 2.08 %- d x by: 1. - WL 1.5406 - Monodinic - a 8.552 - b 13.040 - c 7.200 - alpha 90.000-beta 115.7-gamma90.000-Base

2-Theta - Scale ffilSample 63-1536 - File: Pam_63-1536.RAW - Type: 2Th/Th locked - Start: 5.000 • - End: 70.000 • - Step: 0.020' - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta 5.000 ° - Theta 2.50 Operations: Background 1.000,1.0001 Import (H146-1045 (*)- Quartz, syn - Si02 - Y: 100.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000-gamma 120.000-Primitiv6-P3221 (154)-3-113.01 Qj] 06-0263 (I) -Muscovite-2M1-KAI2(Si3AI)O10(OH,F)2-Y: 12.50 %-dxby: 1.-WL: 1.5406-Monodinic-a5.19-b9.03-c20.05-alpha 90.000-beta 95.77-gamma 90.000-Base-centred-C2/c (15)- Hi) 09-0466 (*)- Albite, ordered - NaAISi308 - Y: 16.67 %- d x by: 1.- WL: 1.5406 - Triclinic - a 8.144 - b 12.787 - c 7.160 - alpha 94.26 - beta 116.6 - gamma 87.67 - Base-centred-C-1 (0)-4-664.837-Mc [029-0701 (I) - dinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si ,AI)4010(OH)8 - Y: 18.75 %- d x by: 1.- WL: 1.5406 - Monodinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.CW0-beta 97.15-gamma 90.000-Basecentred- [019-0002 (I) - Orthoclase, ban an - (K,Ba,Na)(Si,AI)408 - Y: 2.08 %- d x by: 1. - WL: 1.5406 - Monodinic - a 8.552 - b 13.040 - c 7.200 - alpha 90.000 - beta115.7-gamma90.000-Base-centred-C2/m(12) (H05-0586 (*) - Calcite, syn - CaC03 - Y: 2.08 % - d x by: 1. - WL: 1.5406 - Hexagonal (Rh) - a 4.989 - b 4.98900 - c 17.062 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - R-3c (167) - 6 - 367.78 Sample 65-1596

5 10 20 30 40 50 60 7C 2-Theta - Scale BSsample 65-1596 - File: Pam_65-1596.RAW - Type: 2WTh locked - Start: 5.000 • - End: 70.000' - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta 5.000' - Theta 2.50 Operations: Background 1.000,1.0001 Import EH 46-1045 (")- Quartz, syn - Si02 - Y: 70.83 %- d x by: 1.- WL: i.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-P3221 (154)-3-113.010 Qj) 06-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)010(OH,F)2 - Y: 9.03 %- d x by: 1.- WL: 1.5406 - Monoclinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000 - beta 95.77-gamma 90.000-Base-centred-C2/c (15)-4 DUl 09-0466 (*)- Albite, ordered - NaAISi308 - Y: 12.50 %- d xby: 1. -WL 1.5406 -Tridinic - a8.144 - b 12.787 - o 7.160 -alpha 94.26 - beta 116.6-gamma 87.67-Base-centred-C-1 (0)-4-664.837-l/lc ED 29-0701 (I) -Clinochlore-1Mllb, ferroan-(Mg,Fe)6(Si,AI)4O10(OH)8-Y: 12.50 %-dxby: 1.-WL: 1.5406 -Monoclinic-a 5.36-b 9.28-c 14.2-alpha 90.000-beta 97.15-gamma 90.000-Base-centred- tlji05-0586 (") - Calcite, syn - CaC03 - Y: 6.25 % - d x by: 1. - WL: 1.5406 - Hexagonal (Rh) - a 4.989 - b 4.98900 - c 17.062 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - R-3c (167) - 6 - 367.78 Sample 66-136" Greyish Blue

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30 40 2-Theta - Scale ElSample 66-136" Greyish Blue - File: Pam_66-136.RAW - Type: 2TWTh locked - Start: 5.000 • - End: 70.000 • - Step: 0.020 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta 5.000" - Operations: Background 1.000,1.0001 Import ED 30-0662 (*)- Vivianite, syn - Fe3(P04)2-8H20 - Y: 95.83 %- d x by: 1.- WL: 1.5406 - Monodinic - a 10.034 - b 13.449 - o 4.707 - alpha 90.000 - beta 102.65-gamma90.000-Body-centred-l2/m(12)-2- Sample 66-1632"

2-Theta - Scale fflSample 66-1632" - File: Pam_66-1632.RAW - Type: 2Th/Th locked - Start: 5.000 • - End: 70.000 * - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta 5.000 • - Theta 2.50 Operations: Background 1.000,1.0001 Import [046-1045 (*)- Quartz, syn - Si02 - Y: 100.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-P3221 (154)-3-113.01 Qj]06-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,P)2 - Y: 25.00 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000 - beta 95.77 - gamma 90.000 - Base-centred - C2/C (15) - Djlo9-0466(*)-Albite, ordered-NaAISi308-Y: 18.75%-dxby:1.-WL: 1.5406-Tridinic-a8.144-b 12.787-c7.160-alpha94.26-beta 116.6-gamma 87.67-Basecentred-C-1 (0)-4-664.837-l/lc [D29-0701 (I) -Clinxhlore-1Mllb,ferroan-(Mg,Fe)6(Si,AI)4O10(OH)8-Y: 50.00 %-dxby: 1.-WL: 1.5406- Monoclinic-a5.36-b9.28-c14.2-alpha90.000-beta 97.15-gamma90.000-Base-centred- Sample 67-1657"

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IM'l^L

2-Theta - Scale HSample 67-1657' - File: Pam_67-1657.RAW - Type: 2Th/Th locked - Start: 5.000 • - End: 70.000° - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta 5.000" - Theta 2.50 Operations: Background 1.000,1.0001 Import 0346-1045 (•) - Quartz, syn - Si02 - Y: 100.00 % - d x by: 1. - WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P3221 (154) - 3 -113.01 03 06-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 8.33 %- d x by: 1. - WL: 1.5406 - Monoclinic - a 5.19 - b 9.03 - c 20.05 -alpha 90.000-beta 95.77-gamma 90.000-Base-centred-C2/C (15)-4 [009-0466 (')-Albite, ordered - NaAISi308 - Y: 14.75 %-dxby: 1.-WL 1.5406-Tridinic-a8.144-b 12.787-c7.160 -alpha 94.26 -beta 116.6-gamma 87.67- Base-centred - C-1 (0)-4-664.837-l/lc Q329-0701 (I) - Clinochlore-1Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 10.94 % - d xby: 1. - WL: 1.5406 - Monoclinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 -gamma 90.000 - Base-centred - Q305-0586 (•) - Calcite, syn - CaC03 - Y: 2.08 % - d x by: 1. - WL: 1.5406 - Hexagonal (Rh) - a 4.989 - b 4.98900 - c 17.062 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - R-3c (167) - 6 - 367.78 Sample 68-1694"

2-Theta - Scale BSSample 68-1694" - File: Pam_68-1694.RAW - Type: 2Th/Th locked - Start: 5.000 • - End: 70.000 * - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 'C (Room) - Time Started: 0 s - 2-Theta 5.000 ° - Theta 2.50 Operations: Background 1.000,1.0001 Import [HI 46-1045 (*) - Quartz, syn - Si02 - Y: 75.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-P3221 (154)-3-113.010 0306-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 10.42 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000 - beta 95.77 - gamma 90.000 - Base«entred - C2/C (15) - El 09-0466 (*) - Albite, ordered -NaAISi308-Y: 12.50 %-dxby: 1.-WL: 1.5406-Tridinic-a8.144-b12.787-c7.160-alpha 94.26 -beta 116.6-gamma87.67-Base-centred-C-1 (0)-4-664.837-l/lc [029^)701 (I)-Clinochlore-1Mllb,ferroan-(Mg,Fe)6(Si,AI)4O10(OH)8-Y: 14.58 %-d xby: 1.-WL: 1.5406-Monoclinic-a5.36-b 9.28 - c 14.2 - alpha 90.000 -beta 97.15-gamma 90.000- Base-centred- U305-0586 (*) - Calcite, syn - CaC03 - Y: 4.17 % - d x by: 1. - WL: 1.5406 - Hexagonal (Rh) - a 4.989 - b 4.98900 - c 17.062 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - R-3c (167) - 6 - 367.78 ill! 19-0002 (I) - Orlhoclase, barian - (K,Ba,Na)(Si,AI)408 - Y: 2.08 % - d x by: 1. - WL: 1.5406 - Monodinic - a 8.552 - b 13.040 - c 7.200 - alpha 90.000 - beta 115.7 - gamma 90.000 - Base«sntred - C2/m (12) Sample 69-1722"

5 10 20 30 40 50 60 7( 2-Theta - Scafe ffil Sample 69-1722" - File: Pam_69-1722.RAW - Type: 2Th/Th locked - Start: 5.000 ° - End: 70.000 ° - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 *C (Room) - Time Started: 0 s - 2-Theta 5.O0O • - Theta: 2.50 Operations: Background 1.000,1.0001 Import 03 46-1045 (*)- Quartz, syn - Si02 - Y: 100.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-P3221 (154)-3-113.01 HJI 06-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 6.25 %- d x by: 1. - WL: 1.5406 - Monoclinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000 - beta 95.77-gamma 90.000-Base-centred-C2/c (15)-4 Qj] 09-0466 O-Albite, ordered- NaAISi308-Y: 13.02 %-dxby: 1.-WL 1.5406-Tridinic-a8.144-b12.787-c7.160 -alpha 94.26-beta 116.6-gamma 87.67 - Baseântred-C-1 (0)-4-664.837-l/lc QJ29-0701 (I) -Clinochlore-1Mllb,ferroan-(Mg.Fe)6(Si,AI)4O10(OH)8-Y: 12.50 %-dxby: 1.-WL: 1.5406- Monpclinic-a5.36-b9.28-c14.2-alpha90.000-beta97.15-gamma 90.000-Baseêntred- llil 19-O002 (I) - Orthoclase, barian - (K,Ba,Na)(Si,AI)408 - Y: 2.08 % - d x by: 1. - WL 1.5406 - Monoclinic - a 8.552 - b 13.040 - c 7.200 - alpha 90.000 - beta 115.7 - gamma 90.000 - Baseêntred - C2/m (12) Sample 70-1754"

2-Theta - Scale fflsample 70-1754" - File: Pam_70-1754.RAW - Type: 2Th/Th locked - Start: 5.000' - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 'C (Room) - Time Started: 0 s - 2-Theta: 5.000 * - Theta: 2.50 Operations: Background 1.000,1.0001 Import [0 46-1045 (') - Quartz, syn - Si02 - Y: 100.00 % - d x by: 1. - WL: 1.5406 - Hexagonal -a4.91344-b4.91344-c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P3221 (154) - 3 -113.01 |]j]09-O466 (*) - Albite, ordered - NaAISi308 - Y: 20.83 % - d x by: 1. - WL: 1.5406 - Triclinic - a 8.144 - b 12.787 - c 7.160 - alpha 94.26 - beta 116.6 - gamma 87.67 - Base-centred - C-1 (0) - 4 - 664.837 - l/lc Dj]07-0042 (I) - Muscovite-3T - (K,Na)(AI,Mg,Fe)2(Si3.1 AI0.9)O10(OH)2 - Y: 16.67 % - d x by: 1. - WL: 1.5406 - Hexagonal - a 5.203 - b 5.20300 - c 29.988 - alpha 90.000 - beta 90.000 - gamma 120.000 - Pri [1329-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 25.00 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Base-centred - ! Lll47-1743 (C) - Calcite - CaC03 - Y: 2.78 % - d x by: 1. - WL: 1.5406 - Hexagonal (Rh) - a 4.9896 - b 4.98960 - c 17.0610 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - R-3c (167) - 6 - 367.846 Sample 71-1782"

5 10 20 30 40 60 60 7C 2-Theta - Scale HOSample 71-1782" - File: Pam_71-1782.RAW - Type: 2Th/Th looked - Start: 5.000 • - End: 70.000 * - Step: 0.020 ° - Step time: 0.5 s - Temp.: 25 *C (Room) - Time Started: 0 s - 2-Theta: 5.000 • - Theta: 2.50 Operations: Background 1.000,1.0001 Import • H346-1045O-Quartz. syn-Si02-Y: 100.00%-dxby: 1.-WL: 1.5406-Hexagonal-a4.91344-b4.91344-c5.40524-alpha90.000-beta90.000-gamma 120.000-Primitive-P3221 (154)-3-113.01 0306-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 14.67 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.19 - b 9.03 - C20.05 - alpha 90.000 - beta 95.77 - gamma 90.000 - Base-centred - C2/C (15) - HD09-0466C)-Albite, ordered- NaAISi308-Y: 13.20 %-dxby: 1.-WL: 1.5406-Thdinic-a 8.144-b 12.787-c7.160 -alpha 94.26 -beta 116.6 -gamma 87.67- Base-centred - C-1 (0)-4-664.837-l/lc [0129-0701 (I) -aincchlore-1Mllb,fenioan-(Mg.Fe)6(Si,AI)4O10(OH)8-Y: 16.67 %-dxby: 1.-WL: 1.5406-Monodinic-a 5.36-b 9.28-c 14.2-alpha 90.000-beta97.15-gamma90.000-Base-centred- llj!47-1743 (C) - Calcite - CaC03 - Y: 2.08 % - d x by: 1. - WL: 1.5406 - Hexagonal (Rh) - a 4.9896 - b 4.98960 - c 17.0610 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - R-3c (167) -6 - 367.846 Sample 72-1807"

5 10 20 30 40 50 60 7C 2-Theta - Scale fflSample 72-1807" - File: Pam_72-1807.RAW - Type: 2Th/Th locked - Start: 5.000 • - End: 70.000" - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 X (Room) - Time Started: 0 s - 2-Theta 5.000 • - Theta: 2.50 Operations: Background 1.000,1.0001 Import 0346-1045 (*) - Quartz, syn - Si02 - Y: 100.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-PrimiBve-P3221 (154)-3-113.01 009-0466 O-Albite, ordered - NaAISi308- Y: 10.41 %-dxby: 1.-WL: 1.5406-Tridinic-a6.144-b12.787-c7.160-alpha94.26 -beta 116.6 -gamma87.67- Base-centred -C-1 (0)-4-664.837-l/lc D3 06-0263 (I) - Muscovite-2M1 -KAl2(Si3AI)O10(OH,F)2-Y: 10.42 %-dxby: 1.-WL: 1.5406- Monodinic-a5.19-b9.03-c20.05 -alpha 90,000-beta95.77-gamrra 90.000-Base-eentred-C2/c(15)- [ID29-0701 (I) - dinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 -Y: 18.75 % -d x by: 1. -WL: 1.5406 - Monodinic -a5.36-b9.28-c14.2-alpha90.000-beta97.15-gamma90.CK)0-Base««sitred- [U47-1743 (C) - Caltite - CaC03 - Y: 4.17 % - d x by: 1. - WL: 1.5406 - Hexagonal (Rh) - a 4.9896 - b 4.98960 - c 17.0610 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - R-3c (167) - 6 - 367.846 111! 19-0002 (I) - Orthodase, barian - (K,Ba,Na)(Si,AI)408 - Y: 2.08 % - d x by: 1. - WL: 1.5406 - Monodinic - a 8.552 - b 13.040 - c 7.200 - alpha 90.000 - beta 115.7 - gamma 90.000 - Base-centred - C2/m (12) Sample 74-1842

2-Theta - Scale . El Sample 74-1842 - File: Pam_74-1842.RAW - Type: 2Th/Th locked - Start: 5.000 • - End: 70.000 • - Step: 0.020' - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta 5.000 • - Theta 2 Operations: Background 1.000,1.000| Import (U146-1045 (*)- Quartz, syn - Si02 - Y: 100.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-P3221 (154)-3-11 Qj]09-0466 (•) - Albite. ordered - NaAISi308 - Y: 14.58 % - d x by: 1. - WL: 1.5406 - Tridinic - a 8.144 - b 12.787 - c 7.160 - alpha 94.26 - beta 116.6 - gamma 87.67 - Base-centred - C-1 (0) - 4 - 664.837 - US 06-0263 (I) - Muscovite-2M1 - KAl2(Si3AI)O10(OH,F)2 - Y: 14.58 %- d x by: 1.- WL: 1.5406 - Monodinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000-beta 95.77-gamma 90.000-Bas*o8ntred-C2/c(1 [029-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 20.83 % - d x by: 1. - WL: 1.5406 - Monodinic -a 5.36 - b 9.28 - c 14.2 - alpha 90.000 -beta 97.15 - gamma 90.000 - BaseKSntr ILll05-O586 (*)- Calcite. syn - CaC03 - Y: 10.42 %- d x by: 1.- WL: 1.5406 - Hexagonal (Rh) - a 4.989 - b 4.98900 - c 17.062 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-R-3c(167)-6-3 Sample 75-1874

2-Theta - Scale HlSample 75-1874 - File: Pam_75-1874.RAW - Type: 2Th/Th locked - Start: 5.000 • - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 "C (Room) - Time Started: 0 s - 2-Theta: 5.000 • -Theta 2 Operations: Background 1.000,1.0001 Import M 46-1045 (*)- Qjartz, syn - Si02 - Y: 100.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-P3221 (154)-3-11 [ED09-O466 (•) - Albite, ordered - NaAISi308 - Y: 12.50 % - d x by: 1. - WL: 1.5406 - Tridinic - a 8.144 - b 12.787 - c 7.160 - alpha 94.26 - beta 116.6 - gamma 87.67 - Base-centred - C-1 (0) - 4 - 664.837 - EJ 06-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 10.42 %- d x by: 1. - WL: 1.5406 - Monoolinic -a 5.19 - b 9.03 -c 20.05 - alpha 90.000-beta 95.77-gamma 90.000-Base-centred-C2/c(1 [029-0701 (|) - Clinochlore-1 Mllb, ferraan - (Mg.Fe)6(Si,AI)4O10(OH)8 - Y: 16.67 % - d x by: 1. - WL: 1.5406 - Monoolinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Base-centr [ljio50586 (*) - Calcite, syn - CaC03 - Y: 4.17 % - d x by: 1. - WL: 1.5406 - Hexagonal (Rh) - a 4.989 - b 4.98900 - c 17.062 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - R-3c (167) - 6 - 36 Sample 76-1902

CO "c o O 300

2-Theta - Scale fflsample 76-1902 - File: Pam_76-1902.RAW - Type: 2Th/Th locked - Start 5.000 • - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta 5.000 • - Theta: 2 Operations: Background 1.000,1.0001 Import Q346-1045 (')- Quartz, syn - Si02 - Y: 100.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive. P3221 (154)-3-11 El 09-0466 (*)- Albite, ordered - NaAISi308 - Y: 14.58 %- d x by: 1.- WL: 1.5406 - Triclinic - a 8.144 - b 12.787 - c 7.160 - alpha 94.26 - beta 116.6 - gamma 87.67-Base-centred-C-1 (0)-4-664.837- 006^263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 20.83 % - d x by: 1. - WL 1.5406 - Monodinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000 - beta 95.77 - gamma 90.000 - Base-centred - C2fc (1 0329-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 31.25 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.36 - b 9:28-c14.2-a)pha90.000-beta97.15-gamrna 90.000-Base«sntr Qj] 05-0586 (")- Calcite, syn - CaC03 - Y: 4.17 %- d x by: 1.- WL: 1.5406 - Hexagonal (Rh) - a 4.989 - b 4.98900 - c 17.062 - alpha 90.000 - beta 90.000 - gamma 120.000-Primifve-R-3c(167)-6-36 Sample 77-1932

2-Theta - Scale BSsample 77-1932 - File: Pam_77-1932.RAW - Type: 2Th/Th locked - Start: 5.000 ° - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 "C (Room) - Time Started: 0 s - 2-Theta 5.000 • -Theta 2 Operations: Background 1.000,1.0001 Import [Q46-1045 (*) - Quartz, syn-Si02-Y: 97.92 %-dxby: 1.-WL: 1.5406-He)

2-Theta - Scale HlSample 78-1962" - File: Pam_78-1962.RAW - Type: 2Th/Th locked - Start: 5.000" - End: 70.000 ° - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 'C (Room) - Time Started: 0 s - 2-Theta: 5.000 • - Theta 2.50 Operations: Background 1.000,1.0001 Import [1346-1045 (•) -Quartz. syn-Si02-Y: 100.00 %-dxby: 1.-WL: 1.5405- Hexagonal-a4.91344-b4.91344-c5.40524-alpha90.000-beta90.000-gamma 120.000-Primitive-P3221 (154)-3-113.01 GO 06-0263 (I) - Muscovite-2M1 -KAI2(Si3AI)O10(OH,F)2-Y: 12.50 %-dxby: 1.-WL: 1.5406-Monodinic-a5.19-b 9.03 -c20.05-alpha90.000-beta95.77-gamma 90.000-Bas¢ned-C2/c(15). [041-1480 (I) - Albite, calcian, ordered - (Na,Ca)AI(Si,AI)308 - Y: 16.15 % - d x by: 1. - WL: 1.5406 - Tridinic - a 8.161 - b 12.858 - c 7.112 - alpha 93.68 -beta 116.42 - gamma 89.39 - Bas»centred - C-1 (0) - Dj)29-0701 (I) - Qinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 16.67 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Base-centred - 1019-0002 (I) - Orthoclase. barian - (K,Ba,Na)(Si,AI)408 - Y: 2.08 % - d x by: 1. - WL: 1.5406 - Monodinic - a 8.552 - b 13.040 - c 7.200 - alpha 90.000 - beta 115.7 - gamma 90.000 - Base-centred - C2/m (12) Sample 79-1992"

2-Theta - Scale fflSample 79-1992" - Re: Pam_79-1992.RAW - Type: 2Th/Th locked - Start: 5.000 ° - End: 70.000 • - Step: 0.020" - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta 5.000 ° - Theta 2.50 Operations: Background 1.000,1.0001 Import [0)46-1045 (•) -Quartz, syn-Si02-Y: 100.00 %-dxby: 1.-WL: 1.5406- Hexagonal - a 4.91344-b 4.91344-c 5.40524-alpha 90.000 -beta 90.000-gamma 120.000-Primitive-P3221 (154) -3-113.01 Q341-1480 (I) - Albite, calcian, ordered -(Na,Ca)AI(Si,AI)308- Y: 9.72 %-dxby: 1. - WL: 1.5406-Triclinic- a8.161 - b 12.858-c7.112-alpha 93.68-c«ta 116.42-gamma 89.39-Base-centred-C-1 (0)- 03 06-0263 (I) -Muscovite-2M1-KAI2(Si3AI)010(OH,F)2-Y:12.50%-dxby:1.-WL:1.M06-Mon^ 029-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 25.00 % -d x by: 1. - WL 1.5406 - Monoclinic -a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Base-centred - ill! 19-0002 (I) - Orthoclase, barian - (K,Ba,Na)(Si,AI)408 - Y: 2.08 % - d x by: 1. - WL: 1.5406 - Monoclinic - a 8.552 - b 13.040 - c 7.200 - alpha 90.000 - beta 115,7 - gamma 90.000 - Base-centred - C2/m (12) Sample 80-2022"

2-Theta - Scale fflsample 80-2022" - File: Pam_80-2022.RAW - Type: 2Th/Th locked - Start 5.000 ° - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 *C (Room) -Time Started: 0 s - 2-Theta: 5.000 • - Theta 2.50 Operations: Background 1.000,1.0001 Import M 46-1045 (')- Quartz, syn - Si02 - Y: 100.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-P3221 (154)-3-113.01 D341-1480 (I) - Albite, calci an, ordered - (Na,Ca)AI(Si,AI)308 - Y: 50.00 %- d xby: 1. - WL: 1.5406 -Triclinic - a 8.161 - b 12.858 - c 7.112 - alpha 93.68 - beta 116.42-gamma 89.39-Base-centred - C-1 (0). HO 06-0263 (I) - Musccvite-2M1 - KAI2(Si3AI)O10(OH,F)2 -Y: 50.00 %- d x by: 1.- WL: 1.5406 - Monodinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.CXM-beta95.77-gamma90.000-Base-centred-C2/c(15)- [029-0701 (I) -ainochlore-1Mllb,ferroan-(Mg,Fe)6(Si,AI)4010(OH)8-Y: 29.17 %-d xby: 1.-WL: 1.5406- Monodinic-a 5.36-b 9.28 -c14.2-aJp*a90.(K)0-beta97.15-gamrrB 90.000-Base-centred- Hil 19-0002 (I) - Orthoclase. ban an - (K.Ba.Na)(Si,AI)408 - Y: 4.17 %- d x by: 1.- WL: 1.5406 - Monodinic - a 8.552 - b 13.040 - c 7.200 - alpha 90.000-beta115.7-garnma90.000-Base-centred-C2/m(12) Sample 81-2052"

2-Theta - Scale fflsample 81-2052" - File: Pam_81-2052.RAW -Type: 2Th/Th locked - Start: 5.000 • - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s -Temp.: 25 °C (Room) -Time Started: 0 s - 2-Theta 5.000 • -Theta 2.50 Operations: Background 1.000,1.0001 Import Dj] 46-1045 (')- Quartz, syn - Si02 - Y: 100.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-P3221 (154)-3-113.01 (HI 06-0263 (I) - Muscovite-2M1 - KAJ2(Si3fl)010(OH,F)2 - Y: 22.92 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000 - beta 95.77 - gamma 90.000 - Base-centred - C2/C (15)- 0341-1480 (I) -Albite, calcian. ordered -(Na,Ca)AI(Si,AI)308- Y: 11.81 %-dxby: 1.-WL: 1.5406-Tridinic-a8.161-b 12.858 -C7.112 -alpha93.68-beta 116.42-gamma89.39 -Bas¢red-C-1 (0)- D329-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4010(OH)8 - Y: 22.92 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Base-centred - Sample 82-2084"

5 10 20 30 40 50 60 7C 2-Theta - Scale ffilSample 82-2084" - File: Pam_82-2084.RAW - Type: 2Th/Th locked - Start: 5.000 ° - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 "C (Room) - Time Started: 0 s - 2-Theta: 5.000 • - Theta 2.50 Operations: Background 1.000,1.000| Import [Q 46-1045 (*)- Quartz, syn - Si02 - Y: 100.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - o 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-P3221 (154)-3-113.01 G306-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 20.05 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000 - beta 95.77 - gamma 90.000 - Bas&«entred - C2/C (15) - Qj]09-O466 (•) - Albite, ordered - NaAISi308 - Y: 10.42 % - d x by: 1. - WL: 1.5406 - Triclinic - a 8.144 - b 12.787 - c 7.160 - alpha 94.26 - beta 116.6 - gamma 87.67 - Base-centred - C-1 (0) - 4 - 664.837 - l/lc D329-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 29.17 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Base-centred - (ill 19-0002 (I) - Orthoclase, bari an - (K.Ba.Na)(Si,AI)408 - Y: 4.17 %- d xby: 1. -WL 1.5406 - Monodinic - a 8.552 - b 13.040 - c 7.200 - alpha 90.000-beta115.7-gamma 90.000-BaseKaitred-C2/m (12) Sample 83-2112"

2-Theta - Scale HlSample 83-2112" - File: Pam_83-2112.RAW - Type: 2Th/Th locked - Start: 5.0CO • - End: 70.000 ° - Step: 0.020 * - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta 5.000 • -Theta 2.50 Operations: Background 1.000,1.0001 Import [046-1045 (') - Quartz, syn - Si02 - Y: 99.30 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-P3221 (154)-3-113.010 E]06-O263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH.F)2 - Y: 38.27 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000 - beta 95.77 - gamma 90.000 - Basocentred - C2/c (15) - Qj]09-0466(*)-Albite, ordered-NaAISi308-Y: 16.41 %-dxby: 1.-WL 1.5406-Tridinic-a8.144-b12.787-c7.160-alpha94.26-beta116.6-gamma87.67-Base-centred-C-1 (0)-4-664.837-l/lc 0329-0701 (I) - Clinochlore-1 Mllb. ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 56.25 %- d x by: 1. - WL 1.5406 - Monodinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000-beta 97.15-gamma 90.000-Bas^centred- Sample 84-2142"

2-Theta - Scale BSsample 84-2142" - File: Pam_84-2142.RAW - Type: 2Th/Th locked - Start: 5.000 • - End: 70.000 • - Step: 0.020' - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta: 5.000 • - Theta: 2.50 Operations: Background 1.000,1.0001 Import HD 46-1045 (•)- Qjartz, syn - Si02 - Y: 100.00 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-P3221 (154)-3-113.01 Hfl06-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 47.92 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000 - beta 95.77 - gamma 90.000 - Base-centred - C2/C (15) - (L]09-0466O-Albite, ordered- NaAISi308-Y: 18.75 %-dxby: 1.-WL 1.5406-Tridinic-a8.144-b12.787-c7.160 -alpha 94.26-beta 116.6 -gamma 87.67-Base-centred-C-1 (0)-4-664.837-l/Ic D]]29-0701 (I) - dinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 37.50 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Sample 85-2167"

2-Theta - Scale Klsample 85-2167" - File: Pam_85-2167.RAW - Type: 2Th/Th locked - Start: 5.000 ° - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 "C (Room) - Time Started: 0 s - 2-Theta: 5.000 • -Theta 2.50 Operations: Background 1.000,1.0001 Import [0146-1045 (')- Quartz, syn - Si02 -Y: 97.92 %- d x by: 1. - WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 12P.000-Primitive-P3221 (154)-3-113.010 Qj]06-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 18.75 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000 - beta 95.77 - gamma 90.000 - Base

2-Theta - Scale 3 86-2200" - File: Pam_86-220O.RAW - Type: 2TIVTh locked - Start 5.000 • - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta 5.000 • -Theta 2.50 Operations: Background 1.000,1.0001 Import [046-1045 (*)- Quartz, syn - Si02 - Y: 70.83 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000-Primitive-P3221 (154)-3-113.010 Djl 06-0263 (I)-Muscovite-2M1 -KAI2(Si3AI)O10(OH,F)2-Y: 14.58 %-dxby: 1.-WL: 1.M06-Monodinic-a5.19-b9.03-c20.05-alpha90.000-beta95.77-gamma90.000-Base

2-Theta - Scale fflSample 87-2227" - File: Pam_87-2227.RAW - Type: 2Th/Th locked - Start: 5.000' - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 'C (Room) - Time Started: 0 s - 2-Theta: 5.000 * - Theta 2.50 Operations: Background 1.000,1.0001 Import D346-1045 (*)- Quartz, syn - Si02 - Y: 100.00 %- d x by: 1. - WL: 1.5406- Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000-gamma120.O00-Primitive-P3221 (154)-3-113.01 E107-0042 (I) - Muscovite-3T - (K,Na)(AI,Mg,Fe)2(Si3.1AI0.9)O10(OH)2 -Y: 29.17 %- d x by: 1. -WL: 1.5406 - Hexagonal - a 5.203-b 5.20300-c 29.988-alpha 90.000-beta 90.000-gamma 120.000-Pri [Elog-0466 (') - Albite, ordered - NaAISi308 - Y: 12.50 % - d x by: 1. - WL: 1.5406 - Triclinic - a 8.144 - b 12.787 - c 7.160 - alpha 94.26 - beta 116.6 - gamma 87.67 - Base-centred - C-1 (0) - 4 - 664.837 - l/lc [E329-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4O10(OH)8 - Y: 27.08 % - d x by: 1. - WL: 1.5406 - Monodlnic - a 5.36 - b 9.28 - c 14.2 - alpha 90.000 - beta 97.15 - gamma 90.000 - Basecentred - i Ull 9-0002 (I) - Orthoclase, bari an - (K,Ba,Na)(Si,Al)408 - Y: 6.25 %- d x by: 1.- WL: 1.5406 - Monodinic - a 8.552 - b 13.040 - c 7.200 - alpha 90.0O0-beta115.7-gamma90.000-Base-centred-C2/m(12) [Q105-0586 (*) - Calcite, syn - CaC03 - Y: 4.51 % - d x by: 1. - WL: 1.5406 - Hexagonal (Rh) - a 4.989 - b 4.98900 - c 17.062 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - R-3C (167) - 6 - 367.78 Sample 88-2262"

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2-Theta - Scale ElSample 88-2262" - File: Pam_88-2262.RAW - Type: 2Th/Th locked - Start 5.000 ° - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta: 5.000 * - Theta 2.50 Operations: Background 1.000,1.0001 Import H346-1045 (') - Quartz, syn - Si02 - Y: 100.00 % - d x by: 1. - WL: 1.5406 - Hexagonal -a4.91344-b4.91344-o 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P3221 (154) - 3 -113.01 HJ06-0263 (I) - Muscovite-2M1 - KAI2(Si3AI)O10(OH,F)2 - Y: 7.90 % - d x by: 1. - WL: 1.5406 - Monodinic - a 5.19 - b 9.03 - c 20.05 - alpha 90.000 - beta 95.77 - gamma 90.000 - Base-centred - C2/o (15) - 4 Qj] 09-0466 (*)-Albite, ordered-NaAISi308-Y; 8.33 %-dxby: 1.-WL: 1.5406-Tridinic-a8.144-b12.787-c7.160-alpha94.26-beta 116.6 - gamma 87.67 - Base<»ntred - C-1 (0)-4-664.837-WcP [029-0701 (I) -Clinochlore-1Mllb,ferroan-(Mg,Fe)6(Si,AI)4010(OH)8-Y: 12.50 %-dxby: 1.-WL: 1.5406-Monodinic-a 5.36-b 9.28-c 14.2-alpha 90.000-beta 97.15-gamma 90.000-Base^entred- 0319-0002 (I) - Orthoclase, barian - (K,Ba,Na)(Si,AI)408 - Y: 4.17 %- d x by: 1.- WL: 1.5406 - Monodinic - a 8.552 - b 13.040 - c 7.200 - alpha 90.000 - beta 115.7-gamma 90.000-Base-centred-C2/m (12) Sample 89-2292"

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40 50 2-Theta - Scale B3Sample 89-2292" - File: Pam_89-2292.RAW - Type: 2Th/Th locked - Start: 5.000 • - End: 70.000 • - Step: 0.020 • - Step time: 0.5 s - Temp.. 25 "C (Room) - Time Started: 0 s - 2-Theta 5.000 • - Theta 2.50 Operations: Background 1.000,1.0001 Import [D146-1045 (*)- Quartz, syn - Si02 - Y: 92.36 %- d x by: 1.- WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000-gamma120.000-Primitive-P3221 (154)-3-113.010 [Q06-0263 (I) - Musccvite-2M1 - KAI2(Si3AI)O10(OH.F)2-Y: 4.17 %-dxby: 1. -WL: 1.5408-Monoclinic-a 5.19-b 9.03-c 20.05-alpha 90.000-beta 95.77-gamma 90.000- Base-centred-C2/c (15)-4 ED 09-0466 (*)-Albite, ordered -NaAISi 308- Y: 10.42 %-dxby: 1.-WL: 1.5406-Tridinic-a8.144-b12.787-c7.160-alpha94.26-beta116.6-gamma 87.67 - Base-centred-C-1 (0)-4-664.837-Wc [Q 29-0701 (I) - Clinochlore-1 Mllb, ferroan - (Mg,Fe)6(Si,AI)4010(OH)8 - Y: 4.17 % - d x by: 1. - WL: 1.5406 - Monoclinic - a 5.36 - b 9.28 - c 14.2-alpha 90.000-teta 97.15-gamnra 90.000-Base-centred - 111] 19-0002 (I) - Orthoclase, ban an - (K,Ba,Na)(Si,AI)408 - Y: 4.17 %- d x by: 1. - WL 1.5406 - Monoclinic - a 8.552 - b 13.040 - c 7.200 - alpha 90.000 - beta 115.7-gamma 90.000-Base-centred-C2/m (12) Sample 90-2317

vMlji, ,/v'fl.i. |U|Hi r r, I^.M- t ,.| |M>.| f.,n.> A^ 60 2-Theta - Scale KlSample 90-2317 - File: Pam_90-2317.RAW - Type: 2WTh locked - Start: 5.000 • - End: 70.000 • - Step: 0.020g - Step time: 0.5 s - Temp.: 25 "C (Room) - Time Started: 0 s - 2-Theta 5.000 ° - Theta 2.50 Operations: Background 1.000,1.0001 Import G346-1045 (•) - Quartz, syn - Si02 - Y: 100.00 % - d x by: 1. - WL: 1.5406 - Hexagonal - a 4.91344 - b 4.91344 - c 5.40524 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P3221 (154) - 3 -113.01 Q307-0042 (I) - Muscovite-3T - (K,Na)(AI.Mg,Fe)2(Si3.1 AI0.9)O10(OH)2 - Y: 11.46 % - d x by: 1. - WL: 1.5406 - Hexagonal - a 5.203 - b 5.20300 - c 29.988 - alpha 90.000 - beta 90.000 - gamma 120.000 - Pri [U29-0701 (I) -Clincchlore-1Mllb,ferroan-(Mg,Fe)6(Si,AI)4010(OH)8-Y: 9.03 %-dxby: 1.-WL: 1.5406 - Monodinic - a 5.36-b 9.28-c 14.2-alpha 90.000-beta 97.15-gamma 90.000-Base-centred- 041-1480 (I) -AJbite, calcian, ordered - (Na.Ca)M(Si,AI)308 - Y: 24.61 %-dxby: 1.-WL: 1.5406-Triclinic-a 8.161 -b 12.858 -c7.112-alpha93.68-beta116.42-gamma89.39-Base-centred-C-1 (0)- [y 05-0586 (") - Calcite, syn - CaC03 - Y: 26.50 % - d x by: 1. - WL: 1.5406 - Hexagonal (Rh) - a 4.989 - b 4.98900 - c 17.062 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - R-3c (167) - 6 - 367.7 ii,i!l9-O002 (I) - Orthoclase, bari an - (K,Ba,Na)(Si.AI)408 - Y: 8.07 %- d x by: 1. - WL: 1.5406 - Monodinic - a 8.552 - b 13.040 - c 7.200 - alpha 90.000-beta 115.7-gamrra90.OT0-Base-centred-C2/m(12) APPENDIX V

LGSS-ON-IGNITION RESULTS Loss-on-lgnition Results

Depth Crucible Wt. Dry Wt. (100) After burn Wt. (550) LOI m Sed and Crucible Sed and Crucible % 0.381 6.9179 8.8111 8.6953 6.12% 0.4826 7.3514 9.9502 9.8365 4.38% 0.5842 6.7446 8.8147 8.7393 3.64% 0.8382 6.4095 8.9975 8.9171 3.11% 0.9398 7.3415 9.684 9.631 2.26% 1.0414 6.6739 8.8343 8.7554 3.65% 1.143 6.5406 8.6249 8.5546 3.37% 1.2954 7.1448 10.3201 10.2014 3.74% 1.4478 6.7386 10.2203 10.1151 3.02% 1.5494 7.6398 10.305 10.215 3.38% 1.651 6.827 9.5643 9.4871 2.82% 1.7526 7.4307 9.6883 9.6285 2.65% 1.8542 7.9426 10.8449 10.6009 8.41% 1.9558 7.1526 10.5065 10.4223 2.51% 2.0574 6.662 10.5228 10.432 2.35% 2.159 6.5871 8.4536 8.4058 2.56% 2.2606 6.4243 8.4138 8.3548 2.97% 2.3622 7.3629 9.7861 9.7177 2.82% 2.6162 7.597 9.9115 9.8406 3.06% 2.7178 7.5366 10.6858 10.6001 2.72% 2.8194 7.341 10.8768 10.7997 2.18% 2.921 7.333 10.008 9.9456 2.33% 3.0226 6.758 10.4114 10.3303 2.22% 3.1242 7.4301 10.1348 10.0784 2.09% 3.2258 7.4298 10.9782 10.9042 2.09% 3.3274 7.4442 10.8266 10.7562 2.08% 3.429 7.4918 10.7689 10.7023 2.03% 3.5306 7.3123 10.8868 10.8105 2.13% 3.6322 7.5012 10.6034 10.5414 2.00% 4.1402 6.7161 8.6591 8.6217 1.92% 4.2418 6.4555 7.7071 7.6826 1.96% 4.8514 6.533 9.0943 9.0422 2.03% 4.953 7.3293 9.7138 9.667 1.96% 5.0546 6.4937 8.6534 8.6108 1.97% 5.1562 6.7341 9.2162 9.1691 1.90% 5.2578 7.6041 10.344 10.291 1.93% 5.4102 6.529 9.1335 9.0709 2.40% 5.5118 7.0935 9.5267 9.4732 2.20% 5.6134 6.5724 9.162 9.1119 1.93% 5.715 6.76 9.0172 8.975 1.87% 5.8674 7.6097 10.454 10.3997 1.91% 5.969 6.6568 9.873 9.8157 1.78% 6.0706 7.3011 10.4795 10.4193 1.89% 6.1722 6.6143 10.1934 10.1311 1.74% 6.3246 6.7027 9.8002 9.7466 1.73% 6.477 6.8497 11.0112 10.9446 1.60% 6.5786 7.4181 10.7224 10.67 1.59% Loss-on-lgnition Results

Depth Crucible Wt. Dry Wt. (100) After burn Wt. (550) LOI m Sed and Crucible Sed and Crucible % 6.9596 6.4505 9.8285 9.7718 1.68% 7.0612 6.9186 10.0938 10.0463 1.50% 7.1628 7.6401 10.9068 10.8572 1.52% 7.6454 6.7388 10.7668 10.7211 1.13% 7.747 6.5879 9.6857 9.6474 1.24% 7.8486 6.6624 9.6971 9.6531 1.45% 8.1534 6.4099 9.4213 9.3836 1.25% 8.255 7.9426 10.9404 10.898 1.41% 8.3566 7.1452 10.4403 10.3918 1.47% 8.4582 6.744 10.2418 10.1943 1.36% 8.8138 6.8027 11.2794 11.2156 1.43% 8.9154 7.3516 10.4855 10.4408 1.43% 9.017 7.1527 10.7365 10.6845 1.45% 9.1186 6.5407 9.6306 9.5843 1.50% 9.525 6.6743 9.6797 9.6322 1.58% 9.6266 7.4312 10.9948 10.9533 1.16% 9.7282 7.3418 10.6832 10.6362 1.41% 10.033 6.4241 9.4457 9.406 1.31% 10.1346 7.3625 9.4761 9.445 1.47% 10.2362 7.5971 10.1558 10.1156 1.57% 10.3378 7.5363 10.434 10.3877 1,60% 10.8458 7.341 10.1527 10.1123 1.44% 10.9474 7.3328 10.0929 10.0485 1.61% 11.049 6.7578 9.5383 9.5013 1.33% 11.1506 7.4288 10.7938 10.7477 1.37% 11.2522 7.4296 9.8149 9.7797 1.48% 11.3538 7.444 9.7166 9.6828 1.49% 11.4554 7.4916 10.2122 10.167 1.66% 11.557 7.3118 9.7409 9.7062 1.43% 11.9126 7.5006 10.9537 10.9033 1.46% 12.0142 6.7159 9.7844 9.7411 1.41% 12.1158 6.4551 9.0736 9.0355 1.46% 12.5222 6.533 9.312 9.2671 1.62% 12.6238 7.3293 10.9066 10.8655 1.15% 12.7254 6.4934 9.1842 9.1467 1.39% 12.9794 6.734 10.6172 10.5687 1.25% 13.081 7.6038 11.3722 11.322 1.33% 13.1826 6.5288 9.6103 9.568 1.37% 13.2842 7.0935 9.7883 9.7518 1.35% 13.3858 6.5724 9.5922 9.5573 1.16% 14.1478 6.7599 9.7116 9.6616 1.69% 14.2494 7.6097 11.8729 11.8084 1.51% 14.351 6.6569 9.5464 9.5065 1.38% 14.4526 7.3011 10.21 10.1716 1.32% 14.5542 6.6143 9.6675 9.6178 1.63% 15.0622 6.7032 9.6444 9.598 1.58% 15.1638 6.8494 10.4916 10.4456 1.26% Loss-on-lgnition Results

Depth Crucible Wt. Dry Wt. (100) After burn Wt. (550) LOI m Sed and Crucible Sed and Crucible % 15.2146 6.9181 10.3638 10.3191 1.30% 15.2654 7.418 10.4554 10.3963 1.95% 15.3162 7.4914 9.9388 9.8325 4.34% 15.367 6.4511 8.699 8.629 3.11% 15.4178 7.3414 9.6664 9.6125 2.32% 15.4686 6.5871 9.1586 9.102 2.20% 15.5194 6.7158 9.3313 9.2638 2.58% 15.5702 6.7388 10.5504 10.4694 2.13% 15.621 6.4096 9.8333 9.7509 2.41% 15.6718 7.9426 11.6968 11.6089 2.34% 15.7734 7.1448 10.4955 10.4161 2.37% 15.5702 6.6619 9.6821 9.6158 2.20% 15.9766 6.4096 10.4067 10.3146 2.30% 16.0782 6.9182 9.8162 9.7491 2.32% 16.1798 7.1525 10.3719 10.2911 2.51% 16.2814 6.8027 10.2142 10.1384 2.22% 16.383 7.3516 10.8975 10.801 2.72% 16.637 6.7435 10.1098 10.0261 2.49% 16.7386 6.674 9.9619 9.8572 3.18% 16.7894 6.5405 10.6248 10.4975 3.12% 16.891 7.4309 11.1777 11.0622 3.08% 16.9926 7.6395 10.5119 10.4338 2.72% 17.0942 7.3415 10.5017 10.4186 2.63% 17.1958 6.5325 8.8829 8.809 3.14% 17.2974 6.4551 8.4798 8.4253 2.69% 17.399 7.5002 11.4408 11.3357 2.67% 17.5006 7.3115 9.1222 9.0703 2.87% 17.6022 7.4436 9.5607 9.4987 2.93% 17.7038 7.4914 9.0002 8.9625 2.50% 17.8054 7.4293 10.8271 10.7422 2.50% 17.907 6.7159 9.5748 9.4998 2.62% 18.0086 7.4287 10.8936 10.7921 2.93% 18.1102 6.7573 9.3111 9.2426 2.68% 18.2118 7.3402 9.6901 9.6197 3.00% 18.415 7.5359 10.7745 10.7007 2.28% 18.5166 7.5962 10.8918 10.8165 2.28% 18.6182 7.3619 10.7457 10.6628 2.45% 18.7198 7.3322 10.114 10.0367 2.78% 18.8214 6.4239 8.7612 8.6911 3.00% 18.923 6.8492 9.6727 9.5945 2.77% 19.0246 7.6095 10.4613 10.3906 2.48% 19.1262 6.7025 9.5116 9.4309 2.87% 19.3294 7.4178 10.0813 10.0065 2.81% 19.3802 7.3323 10.6019 10.5157 2.64% • 19.431 7.301 10.1402 10.0675 2.56% 19.4818 7.3402 10.5045 10.4201 2.67% 19.5326 7.4288 10.2707 10.1942 2.69% Loss-on-lgnition Results

Depth Crucible Wt. Dry Wt. (100) After burn Wt. (550) LOI m Sed and Crucible Sed and Crucible % 19.5834 6.5288 9.76 9.6737 2.67% 19.6342 6.674 9.1681 9.0892 3.16% 19.685 6.7598 9.1296 9.066 2.68% 19.7866 6.5722 9.5669 9.481 2.87% 19.8882 7.6035 10.961 10.8626 2.93% 19.9898 6.6566 9.9795 9.8544 3.76% 20.0914 6.4931 10.363 10.2701 2.40% 20.193 7.0931 9.6913 9.6085 3.19% 20.2946 6.7339 9.2978 9.2194 3.06% 20.3962 6.4503 8.4684 8.4008 3.35% 20.4978 7.3514 10.2127 10.1232 3.13% 20.5994 6.5871 8.4906 8.4336 2.99% 20.701 7.4308 10.4906 10.3999 2.96% 20.8026 7.1451 9.7054 9.6308 2.91% 20.9042 6.7436 8.9648 8.9001 2.91% 21.0058 6.6743 8.2519 8.204 3.04% 21.1074 6.7384 8.7516 8.6922 2.95% 21.209 7.6396 9.69 9.6209 3.37% 21.3106 7.9424 10.0209 9.9551 3.17% 21.5646 6.6619 9.1779 9.1021 3.01% 21.6662 6.5406 9.9799 9.8776 2.97% 21.7678 7.1524 9.5749 9.5057 2.86% 21.8694 6.9182 9.9726 9.8729 3.26% 22.225 6.4096 9.4127 9.3258 2.89% 22.3266 6.8025 10.0852 9.9874 2.98% 22.4282 7.3413 10.5303 10.4392 2.86% 22.5298 7.5002 10.7995 10.6978 3.08% 22.8854 6.7159 9.0309 8.9687 2.69% 22.987 7.5963 10.4363 10.3508 3.01% 23.1902 6.7569 8.8806 8.8152 3.08% 23.2918 7.5353 9.7594 9.6913 3.06% 23.3934 6.5326 8.9169 8.8472 2.92% 23.5966 7.3401 9.8365 9.7659 2.83% 23.495 7.3622 9.4987 9.4298 3.22% 23.6982 7.4915 9.0836 9.0372 2.91% 23.7998 6.4552 8.271 8.2186 2.89% 23.9014 6.4238 7.7115 7.6719 3.08% 24.003 7.3117 8.5345 8.4944 3.28% 24.0538 7.4288 8.9655 8.9153 3.27% 24.1046 7.3323 9.039 8.9892 2.92% 24.2062 7.4295 8.642 8.6025 3.26% 24.3078 7.4437 8.7106 8.6703 3.18% 24.4602 6.7599 9.4425 9.3662 2.84% 24.5618 7.0934 8.5535 8.5099 2.99% 24.6634 6.7338 8.0541 8.0175 2.77% 24.7142 7.418 9.0248 8.9803 2.77% 24.8158 6.8494 9.4114 9.3274 3.28% Loss-on-lgnition Results

Depth Crucible Wt. Dry Wt. (100) After burn Wt. (550) LOI m Sed and Crucible Sed and Crucible % 24.8666 7.3011 9.4156 9.3521 3.00% 24.9174 7.6037 9.2382 9.1916 2.85% 25.019 7.6096 8.7713 8.7334 3.26% 25.1206 6.614 7.8266 7.7938 2.70% 25.2222 7.3289 8.9494 8.9019 2.93% 25.3238 6.4931 8.0026 7.9579 2.96% 25.3746 6.7027 8.5545 8.4896 3.50% 25.4762 6.5723 7.9336 7.8955 2.80% 25.5778 6.5288 8.5881 8.5272 2.96% 25.9842 6.6568 8.6414 8.5781 3.19% 26.0858 6.4504 9.0938 9.0196 2.81% 26.1874 6.5873 9.3628 9.2746 3.18% 26.2636 6.5407 8.2896 8.2394 2.87% 26.3652 6.7385 8.8154 8.769 2.23% 26.4668 7.3416 9.3565 9.299 2.85% 26.5176 7.9427 9.973 9.9184 2.69% 26.6192 7.431 8.7232 8.6883 2.70% 26.6954 7.1526 8.9314 8.8822 2.77% 26.797 6.9183 8.9689 8.9077 2.98% 26.8478 7.6397 10.2246 10.1534 2.75% 26.9494 7.1447 9.2484 9.1876 2.89% 27.051 6.674 8.3849 8.3351 2.91% 27.1526 6.8027 8.4482 8.4047 2.64% 27.2542 6.4097 8.3348 8.2804 2.83% 27.3558 6.7439 7.9972 7.9646 2.60% 27.4574 6.6619 8.0231 7.9823 3.00% 27.559 7.3516 8.7407 8.6962 3.20% 27.6606 7.3323 8.9607 8.9102 3.10% 27.7622 7.3621 8.9951 8.9455 3.04% 27.8638 6.7159 7.8742 7.8349 3.39% 27.9654 7.5962 9.028 8.9867 2.88% 28.1686 7.3402 9.2188 9.1598 3.14% 28.2702 6.4236 8.0572 8.0094 2.93% 28.3718 6.7575 9.1335 9.0596 3.11% 28.4734 7.5003 9.2848 9.23 3.07% 28.575 7.4915 9.6099 9.5424 3.19% 28.829 7.3118 9.2062 9.1459 3.18% 28.9306 7.4286 . 8.9823 8.9286 3.46% 28.9814 7.4434 9.5258 9.4575 3.28% 29.083 6.5327 8.6108 8.5428 3.27% 29.1846 6.455 8.2114 8.1539 3.27% 29.337 7.4296 8.9025 8.8602 2.87% 29.4386 7.5359 9.5238 9.4647 2.97% 29.5402 6.6138 7.9122 7.868 3.40% 29.591 6.7599 8.4803 8.4274 3.07% 29.6926 7.6037 9.5637 9.4991 3.30% 29.7942 7.6093 10.3468 10.2614 3.12% Loss-on-lgnition Results

Depth Crucible Wt. Dry Wt. (100) After burn Wt. (550) LOI m Sed and Crucible Sed and Crucible % 29.8958 7.3009 9.7572 9.676 3.31% 29.9974 6.6567 9.6611 9.5658 3.17% 30.099 7.0932 10.3488 10.2428 3.26% 30.2006 6.8491 9.1601 9.0809 3.43% 30.2514 6.4502 8.4466 8.3833 3.17% 30.353 6.7029 9.4373 9.3471 3.30% 30.4546 7.4178 10.4168 10.3187 3.27% 30.5054 6.5285 8.5359 8.4666 3.45% 30.607 6.5722 9.2203 9.1319 3.34% 30.7086 7.329 9.6734 9.5936 3.40% 30.8102 6.493 9.7197 9.614 3.28% 30.9118 6.7338 9.254 9.1678 3.42% 31.0134 6.6741 8.7942 8.7218 3.41% 31.4706 7.1453 9.2891 9.2183 3.30% 31.5722 7.3415 9.2313 9.1705 3.22% 31.6738 6.4097 8.6096 8.5366 3.32% 31.7246 6.8027 9.1877 9.1049 3.47% 31.8262 6.7439 8.6714 8.6075 3.32% 31.9278 6.5871 8.5483 8.4875 3.10% 32.1564 7.431 9.1507 9.0977 3.08% 32.2326 6.9185 8.8682 8.8121 2.88% 32.3342 7.3518 8.8529 8.8025 3.36% 32.4358 6.662 7.8408 7.8041 3.11% 32.5374 7.1524 8.2474 8.2102 3.40% 32.639 7.9425 10.1835 10.1093 ' 3.31% 32.7406 6.7386 8.5146 8.4573 3.23% 32.9438 7.6397 9.5385 9.4778 3.20% 33.0454 6.5405 8.0984 8.0477 3.25% 33.147 6.6738 7.6678 7.6359 3.21% 33.2486 7.3515 9.01.33 8.9617 3.11% 33.3502 6.7435 8.2863 8.2336 3.42% 33.4518 6.8028 8.5093 8.4455 3.74% 33.6042 7.6396 9.5617 9.4905 3.70% 33.7058 6.5404 7.9153 7.8657 3.61% 33.8074 6.7385 8.3868 8.3239 3.82% 33.909 7.1451 8.7128 8.6607 3.32% 34.0106 7.5361 9.7033 9.624 3.66% 34.1122 6.424 8.8835 8.8021 3.31% 34.2138 7.3324 8.6285 8.5848 3.37% 34.5186 7.5965 9.3305 9.2708 3.44% 34.6202 6.4551 8.6053 8.5377 3.14% 34.7218 7.4288 9.4517 9.3883 3.13% 34.8234 7.3404 9.0161 8.963 3.17% 34.925 7.4439 8.8125 8.7683 3.23% 35.0266 7.3619 9.4644 9.3991 3.11% 35.1282 7.5006 10.1522 10.0776 2.81% 35.2298 7.4916 9.3058 9.2498 3.09% Loss-on-lgnition Results

Depth Crucible Wt. Dry Wt. (100) After burn Wt. (550) LOI m Sed and Crucible Sed and Crucible % 35.3314 6.7576 9.1741 9.0937 3.33% 35.433 7.4294 8.6768 8.6368 3.21% 35.5346 6.716 8.5361 8.4717 3.54% 35.6362 7.3118 9.1802 9.1204 3.20% 35.7378 6.5327 8.3208 8.2656 3.09% 36.195 6.6618 8.4159 • 8.3591 3.24% 36.2966 6.5875 9.0331 8.9563 3.14% 36.3982 7.3415 9.5628 9.4953 3.04% 36.4998 7.1522 9.479 9.4031 3.26% 36.7538 6.9182 9.2575 9.184 3.14% 36.8554 7.9429 10.1964 10.1245 3.19% 36.957 7.4308 9.8941 9.8152 3.20% 37.0586 6.4098 8.5034 8.435 3.27% 37.1602 7.6095 9.5297 9.4682 3.20% 37.2618 7.3009 9.6514 9.5802 3.03% 37.6174 6.7596 8.3285 8.28 3.09% 37.719 7.0934 8.9379 8.8809 3.09% 37.8206 6.8494 8.6959 8.6304 3.55% 37.9222 6.5724 7.6672 7.6349 2.95% 38.0238 6.6569 8.0319 7.9843 3.46% 38.2778 7.6036 9.1238 9.0739 3.28% 38.3794 7.3288 8.7588 8.7133 3.18% 38.481 6.4503 8.3563 8.2991 3.00% 38.5826 6.7337 8.6012 8.5461 2.95% 38.735 6.5288 7.5951 7.5621 3.09% 38.8366 7.4178 10.141 10.0557 3.13% 39.0906 6.7027 7.9043 7.8739 2.53% 39.1922 6.6141 8.2783 8.2306 2.87% 39.2938 6.7389 8.4983 8.4386 3.39% 39.3954 7.3436 8.8931 8.8468 2.99% 39.497 7.3521 9.4502 9.3754 3.57% 39.5478 6.7575 9.0532 8.9745 3.43% 39.5986 6.7442 9.1525 9.0801 3.01% 40.9194 7.1527 8.3595 8.3155 3.65% 40.9702 6.5409 7.5946 7.5568 3.59% 41.021 7.4308 8.9015 8.8495 3.54% 41.0718 7.4292 8.7246 8.6792 3.50% 41.2242 6.4551 7.2296 7.2027 3.47% 41.3258 6.68 8.1279 8.0756 3.61% 41.4274 6.4246 7.6553 7.6109 3.61% 41.529 7.335 8.3716 8.3341 3.62% 41.6306 7.1448 8.3944 8.3481 3.71% 41.7322 7.4437 8.2106 8.1821 3.72% 41.8338 7.5359 8.847 8.7987 3.68% 42.2656 7.6411 8.6654 8.6313 3.33% 42.2402 7.5962 8.4065 8.3793 3.36% 42.3418 6.8075 7.8498 7.8129 3.54% Loss-on-lgnition Results

Depth Crucible Wt. Dry Wt. (100) After burn Wt. (550) LOI m Sed and Crucible Sed and Crucible % 42.4434 7.3515 8.569 8.524 3.70% 42.545 6.7437 7.8308 7.7934 3.44% 42.6466 6.7386 8.0782 8.0362 3.14% 42.8498 7.4287 8.6856 8.6452 3.21% 42.9514 7.1449 8.4477 8.4032 3.42% 43.053 7.4435 9.1936 9.1355 3.32% 43.1546 6.4551 7.735 7.69 3.52% 43.2562 6.6739 8.0472 7.9988 3.52% 43.3578 6.5406 8.859 8.779 3.45% 43.6118 6.4239 7.6638 7.6234 3.26% 43.7134 7.3323 8.9265 8.8754 3.21% 43.815 7.3403 8.6991 8.6466 3.86% 43.9166 7.5963 9.3031 9.2523 2.98% 44.0182 6.8027 8.2057 8.1617 3.14% 44.1198 7.6397 8.9252 8.8858 3.06% 44.323 7.536 8.8233 8.7785 3.48% 44.4246 7.4303 9.2626 9.2034 3.23% 44.5262 6.7571 8.0787 8.0323 3.51% 44.6278 7.4311 9.2685 9.2064 3.38% 44.7294 7.3649 9.118 9.0591 3.36% 44.831 7.3413 9.0379 8.9822 3.28% 44.9326 7.9423 9.389 9.3354 3.70% 45.1866 6.5871 7.9736 7.9313 3.05% 45.2882 6.9195 8.6045 8.5529 3.06% 45.3898 7.1526 8.632 8.582 3.38% 45.4914 7.3117 8.9193 8.8708 3.02% 45.593 7.5004 8.632 8.6002 2.81% 45.6946 6.5327 7.9081 7.8576 3.67% 45.8978 6.4097 8.0979 8.0465 3.04% 45.9994 6.7157 7.751 7.7193 3.06% 46.101 6.6619 7.4571 7.43 3.41% 46.2026 7.4917 8.7249 8.6806 3.59% 46.3042 6.8494 8.1528 8.1068 3.53% 46.4058 7.6093 10.6278 10.5266 3.35% 46.5582 6.7627 9.871 9.7724 3.17% 46.6598 7.329 8.8216 8.7677 3.61% 46.7614 6.659 7.9553 7.9096 3.53% 46.863 6.4506 7.762 7.7182 3.34% 46.9646 7.3008 8.082 8.0561 3.32% 47.0662 6.5296 8.2386 8.1813 3.35% 47.1678 6.6144 7.9751 7.9303 3.29% 47.4472 7.6048 8.9844 8.9366 3.46% 47.5488 7.4176 8.6382 8.5967 3.40% 47.6504 6.5733 7.6804 7.6403 3.62% 47.752 6.7338 8.0014 7.9554 3.63% 47.8536 7.0971 8.582 8.5315 3.40% 47.9552 6.7027 8.088 8.0384 3.58% Loss-on-lgnition Results

Depth Crucible Wt. Dry Wt. (100) After burn Wt. (550) LOI m Sed and Crucible Sed and Crucible % 48.2346 7.5358 10.0553 9.9759 3.15% 48.3362 6.7436 7.9898 7.9493 3.25% 48.4378 6.4237 8.5756 8.5046 3.30% 48.5394 6.7386 8.707 8.6431 3.25% 48.641 7.6395 9.4286 9.3689 3.34% 48.7426 7.3402 9.0555 8.9976 3.38% 49.0474 6.4549 7.5038 7.4649 3.71% 49.149 6.6739 8.2431 8.1827 3.85% 49.2506 6.8027 8.233 8.181 3.64% 49.3522 7.3515 8.0869 8.0609 3.54% 49.4538 7.3322 8.2511 8.2162 3.80% 49.7078 7.5961 9.1858 9.1288 3.59% 49.8094 7.4434 9.2737 9.2096 3.50% 49.911 7.4287 8.962 8.9094 3.43% 50.0126 6.5403 8.1337 8.0783 3.48% 50.1142 7.1447 8.277 8.2326 3.92% 50.2158 7.429 9.4639 9.3913 3.57% 50.3174 7.4919 9.0807 9.0247 3.52% 50.419 7.9423 9.3085 9.2612 3.46% 50.5206 6.92 8.6037 8.5413 3.71% 50.6222 7.3414 8.8975 8.8392 3.75% 50.7238 7.5004 9.1426 9.0848 3.52% 50.8254 6.5872 8.1166 8.06 3.70% 50.927 7.3115 8.7007 8.6476 3.82% 51.0286 6.4095 7.8082 7.7571 3.65% 51.2826 7.1526 9.1919 9.1144 3.80% 51.3842 6.5325 8.0063 7.9528 3.63% 51.4858 7.3619 9.6299 9.5418 3.88% 51.5874 6.7573 8.5117 8.4498 3.53% 51.689 6.6622 7.9634 7.9115 3.99% 51.7906 7.431 8.6948 8.6436 4.05% 51.9938 6.718 8.4301 8.3553 4.37% 52.197 6.849 8.492 8.4211 . 4.32% 52.2986 6.6576 9.0938 8.9937 4.11% 52.4002 6.7596 7.8671 7.8235 3.94% 52.5018 7.3287 8.979 8.908 4.30% 52.705 6.7336 7.6034 7.5657 4.33% 52.8066 7.0932 8.8866 8.8122 4.15%. , 52.9082 6!6139 7.9574 7.8999 4.28% 53.0098 7.3009 8.8278 8.7607 4.39% 53.1114 7.6121 9.623 9.5359 4.33% 53.213 6.572 9.3457 9.2287 4.22% 53.3146 7.6036 10.3689 10.2483 4.36% 53.5178 6.45 9.8449 9.6892 4.59% 53.6194 6.5286 8.5106 8.4185 4.65% 53.721 7.4177 9.7961 9.6861 4.62% 53.8226 7.5961 9.5295 9.4376 4.75% Loss-on-lgnition Results

Depth Crucible Wt. Dry Wt. (100) After burn Wt. (550) LOI m Sed and Crucible Sed and Crucible % 53.9242 6.6738 9.8284 9.6851 4.54% 54.0258 7.3514 10.4497 10.3085 4.56% 54.2798 6.7437 10.4967 10.3211 4.68% 54.3814 6.5405 10.6246 10.4371 4.59% 54.483 6.7384 9.6968 9.5614 4.58% 54.5338 6.5873 9.8631 9.7128 4.59% 54.5846 7.5358 10.5515 10.416 4.49% 54.6354 7.5003 10.6882 10.5413 4.61% 54.737 7.3623 10.8643 10.7297 3.84% 54.7878 6.4238 8.404 8.3337 3.55% 54.8386 7.9426 10.369 10.2908 3.22% 55.0926 7.4435 10.6562 10.5482 3.36% 55.1942 6.4551 8.5227 8.4493 3.55% 55.2958 7.4288 10.4218 10.3239 3.27% 55.3974 6.8026 8.8338 8.7715 3.07% 55.499 7.6398 10.5418 10.4457 3.31% 55.6006 7.3403 9.4308 9.36 3.39% 55.8038 7.3329 9.9351 9.862 2.81% 55.9054 7.9424 10.4642 10.3864 3.09% 56.007 7.5003 11.3316 11.2066 3.26% 56.1086 7.3414 10.2893 10.1821 3.64% 56.2102 6.5872 9.2249 9.1316 3.54% 56.3118 6.9181 9.1738 9.1017 3.20% 56.7182 6.7159 8.7114 8.6579 2.68% 56.8198 6.4096 7.5347 7.5008 3.01% 56.9214 6.6618 9.3658 9.2826 3.08% 57.023 7.3621 9.9791 9.8902 3.40% 57.1246 7.4311 10.4331 10.3322 3.36% 57.2516 7.1527 9.2672 9.2005 3.15% 57.3024 6.7574 8.7682 8.7039 3.20% 57.404 7.4293 8.8251 8.7822 3.07% 57.5056 7.3117 9.3678 9.304 3.10% 57.6072 6.5328 9.0355 8.9619 2.94% 57.7088 7.4915 9.9805 9.9002 3.23% 57.8104 7.6093 10.0929 10.0163 3.08% 57.912 6.849 8.1457 8.1064 3.03% 58.1152 6.7597 8.7852 8.7353 2.46% 58.2168 7.3285 9.2817 9.2536 1.44% 58.3184 6.7338 7.9321 7.9131 1.59% 58.42 6.614 7.6666 7.6497 1.61% 58.5216 6.6568 7.9306 7.9034 2.14% 58.6232 7.0931 9.1606 9.1035 2.76% 58.8264 7.6037 10.1405 10.106 . 1.36% 58.928 7.4178 8.8376 8.8202 1.23% 59.0296 6.4502 7.0857 7.0676 2.85% 59.1312 7.3009 8.0521 8.0285 3.14% 59.182 6.4552 10.6598 10.5874 1.72% OlOIOlOlCTlUlOlOlOlOl a o roM-^opppo (D (A G>COCOCOCOCOCOCOCOCOCO (A 3 •a U101>I010SM>I P co co bo^^cQcncohoho ••* 0 0)-»0)0)-»-'-»«OlU 3" 6 uioroo)Ms.Mv) StOCXISfflOlCOMJiOOM 00M000000.fc.hOO> 3 -i^o>c»ro^.c»N)^N}Oo o C0OI\3.p*C0 cr 3 WSNCD0000NUOXD C0O)-»OlCI100WM l-JO)->IC7>->l SN3A-KDCO00-' M § C

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M O O 1*0 -»• - NJISJ-XCOCOCO-'O-'CO-ÔICOOOCDNJCO^NI I O a>^.oo-»-ôcnoo)0>MOi*>.*.ooî vP — APPENDIX VI

ION CHROMOGRAPHY RESULTS Ion Chromatography Results

Sample Corrected Correcte Depth Water Chloride Bromide CI/Br ratio Chloride Bromide CI/Br rati (meter) Content (mq/L) (mq/L) (mq/L) (mq/L) 0.3048 29.65 1.10 0.08 14.1 7.407 0.526 14.08 0.9652 37.77 0.46 0.16 2.8 2.425 0.871 2.78 1.4224 37.13 0.91 0.29 3.2 4.894 1.535 3.19 1.7272 33.51 2.15 0.11 20.2 12.843 0.635 20.23 2.032 29.24 2.46 0.10 23.9 16.801 0.703 23.90 2.3368 31.35 3.84 0.05 70.8 24.484 0.346 70.77 2.5654 33.45 2.63 0.06 43.3 15.743 0.364 43.29 2.794 36.43 2.91 0.11 25.5 15.962 0.625 25.54 3.2004 34.6 3.27 <0.05 18.916 3.3528 32.96 2.60 <0.05 15.755 3.5052 33.07 2.80 <0.05 16.951 5.9944 29.14 5.75 <0.05 39.441 6.1468 31.69 3.76 <0.05 23.726 6.2992 34.15 3.66 <0.05 21.415 6.4516 33.35 9.24 nd 55.425 6.5532 30.78 6.95 nd 45.149 8.6868 22.53 5.44 nd 48.321 16.5354 35.39 0.89 0.08 11.7 5.019 0.430 11.67 16.7894 29.79 0.64 0.11 5.9 4.296 0.724 5.93 17.2212 32.37 1.17 0.10 12.0 7.210 0.603 11.95 17.3736 29.2 1.68 0.11 15.0 11.531 0.767 15.03 17.526 29.83 1.53 0.09 17.9 10.271 0.574 17.91 17.8054 30.42 2.59 0.12 21.7 17.031 0.785 21.69 18.034 27.12 8.71 0.09 91.7 64.253 0.700 91.74 19.05 32.13 18.08 0.11 . 158.7 112.512 0.709 158.74 19.2024 30.89 0.95 0.12 7.7 6.176 0.798 7.74 19.3548 33.22 0.75 0.14 5.3 4.502 0.850 5.30 19.685 32.15 1.35 0.14 9.6 8.383 0.873 9.61 19.9136 30.76 2.44 0.17 14.4 15.858 1.105 14.35 20.2438 32.45 2.02 0.24 8.3 12.420 1.496 8.30 20.8788 36.68 12.64 0.12 106.3 68.931 0.649 106.29 21.0312 33.75 8.69 0.14 64.4 51.488 0.800 64.35 21.1836 31.81 14.64 0.15 96.5 92.043 0.954 96.51 21.4884 34.75 18.11 0.15 117.4 104.250 0.888 117.39 21.6408 31.98 21.83 0.20 108.3 136.528 1.260 108.32 22.0726 33.98 8.47 0.14 60.3 49.870 0.828 60.25 22.1996 37.28 9.85 0.18 54.3 52.851 0.972 54.35 22.7076 32.31 12.45 0.20 63.7 77.055 1.210 63.66 23.3426 30.24 11.19 0.23 49.3 73.984 1.501 49.29 23.5204 29.1 9.30 0.17 53.7 63.892 1.190 53.71 23.6982 30.46 7.18 0.16 44.4 47.171 1.062 44.41 23.9522 31.78 32.33 0.19 168.7 203.461 1.206 168.75 24.13 31.2 36.88 0.23 161.1 236.423 1.468 161.07 24.3078 31.5 37.93 0.28 134.6 240.819 1.789 134.61 24.5364 30.04 34.55 0.23 148.0 230.019 1.554 148.00 24.6888 29.81 30.21 0.21 141.4 202.690 1.434 141.39 24.8412 32.83 1.86 0.21 9.0 11.348 1.258 9.02 25.2984 31.57 20.19 0.22 91.8 127.895 1.393 91.82 25.5524 33.75 25.15 0.27 94.4 149.044 1.578 94.42 26.3398 28.03 18.93 0.20 96.3 135.101 1.403 96.27 26.4668 31.2 16.25 0.18 92.1 104.196 1.131 92.12 26.7208 30.12 16.21 0.28 58.9 ' 107.644 1.828 58.87 26.9748 35.86 6.38 0.14 44.5 35.570 0.800 44.46 27.1272 34.1 5.94 0.14 41.1 34.836 0.848 41.09 27.2796 37.84 10.35 0.21 49.3 54.681 1.110 49.26 27.432 35.19 8.48 0.20 43.0 48.194 1.122 42.97 27.5844 38.38 8.74 0.19 47.1 45.541 0.966 47.15 27.7368 40.87 6.71 0.16 40.8 32.860 0.805 40.84 27.8892 35.52 12.08 0.26 47.3 67.996 1.438 47.30 28.0416 34.43 8.10 0.19 42.5 47.056 1.106 42.53 28.194 28.17 4.81 0.15 32.2 34.181 1.060 32.25 28.3464 32.36 12.48 0.26 48.3 77.154 1.599 48.25 28.8036 39.32 11.49 0.23 49.2 58.424 1.188 49.17 OiOiaitTJOi4^J^^^^4^^^4^^4^^4^^4^^4^^^^^4^^^J^^^4^4^W CO CO UUUUUO)WCOUW«WUWN)IOM cocnwwbicocni\}co^^w!^^co^(3>bco^w CO^ComC2^WWOODNl(O^W(D01^0lSWMOCO^WÎCOCn>ISWMOCOO)^S^hOMOCDO)NÎV3S(nMOWOODWÔOOT HI 4^hjoo4^030D^N3034^ôôo4^rooo^cj)ooMoo4^â)03a>c»03ooa)ro»

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